Synthesis of functional microcapsules containing suspensions responsive to electric fields

A sort of functional microcapsules, which contain a suspension responsive to electric fields, is prepared by in situ polymerization of urea and formaldehyde. The suspension is made up of pigment phthalocyanine green (PPG) and tetrachloroethylene. In order to solve the particles' separation from the suspension during the microencapsulation and to obtain microcapsules applying to electronic ink display, the dispersibility of the particles, the contact angles between the particles and the tetrachloroethylene, and the influences of different emulsifiers on the microencapsulation are investigated. It is found that the dispersion extent and lipophilicity of the PPG particles are improved due to their surface modification with octadecylamine. The contact angles between the modified PPG particles and the tetrachloroethylene increase, and the PPG particles modified with 2 wt% octadecylamine have the best affinity for tetrachloroethylene. The interfacial tension between C(2)Cl(4) and H(2)O with urea-formaldehyde prepolymer descends from 43 to 35 mN/m, which indicates that the polymer has certain surface activity. However, water-soluble emulsifiers have an important influence during the microencapsulation because they can absorb on the surfaces of internal phase and prevent the resin of urea-formaldehyde from depositing there. From the SEM images of shell surface and cross section, the microcapsules have relatively smooth surfaces and the average thickness is about 4.5 mum. When the microcapsules are prepared with agitation rates of 1000 and 600 rpm, the mean diameters of the obtained microcapsules are 11 and 155 mum, respectively. The particles in the capsules move toward positive electrode with a responsive time of several hundred milliseconds while providing an electric field.     

Rapid and sensitive determination of ephedrine and pseudoephedrine by micellar electrokinetic chromatography with on-line regenerating covalent coating

A rapid, sensitive and reproducible micellar electrokinetic chromatographic method using hexamethyldisilazane as on-line regenerating covalent coating was developed for the quantification of ephedrine (E) and pseudoephedrine (PE). E and PE were derivatized with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazol for laser-induced fluorescence detection. The on-line regenerating covalent coating formed a combinative double coating with the subsequently produced dynamic SDS coating. The total coating can be easily removed and conveniently regenerated on-line. The simple coating procedure was described. By a series of optimization, a running buffer of 20 mm Na(2)B(4)O(7) + 16 mm SDS was applied for the separation of the derivatives. Linear relationships for E and PE were obtained in the range of 0.044-6.60 microg mL(-1) (correlation coefficients: 0.9975 for E, 0.9981 for PE), and the detection limits for E and PE were 1.71 and 0.67 ng mL(-1), respectively. The separation speed, the reproducibility and the sensitivity were much improved over those of other capillary electrophoresis methods more recently reported. The method was applied to the analysis of the two alkaloids in traditional herbal preparations with recoveries in the range 92.8-104.8%.     

Separation and determination of carnosine-related peptides using capillary electrophoresis with laser-induced fluorescence detection

A capillary electrophoresis (CE) method with laser-induced fluorescence (LIF) detection was developed for the separation and detection of carnosine-related peptides (carnosine, anserine, and homocarnosine). A sensitive and fluorogenic regent, 3-(4-carboxybenzoyl) quinoline-2-carboxaldehyde (CBQCA) was selected as a precapillary labeling reagent for imidazole dipeptides to form isoindole derivatives. The optimized molar ratio between CBQCA and peptide was found to be 75:1, and 50 mmol/L borate buffer (pH 9.2) was used for the derivatization in order to achieve good efficiency. Three imidazole dipeptides were baseline-separated within 20 min by using 112 mmol/L sodium borate (pH 10.4-10.8) as running buffer. Concentration detection limits (signal-to-noise ratios) for carnosine, anserine, and homocarnosine were 4.73, 4.37, and 3.94 nmol/L, respectively. This method has been applied to the analysis of human cerebrospinal fluid (CSF) and meat dry powder of pig and sheep. Recoveries were in the range of 82.9-104.8% for homocarnosine in CSF. For carnosine and anserine, the recoveries are 98.3% and 80.2% in meat dry powder of pig and 111.2% and 112.8% in meat dry powder of sheep, respectively.     

Grafting of 4‐Vinyl Pyridine onto Nylon‐6 Initiated by Cu(III)

In this article, the graft copolymerization of 4‐vinyl pyridine (4VP) onto nylon‐6 (PA6) using potassium diperiodacuprate (III) (DPC)–PA6 redox system as initiator is investigated in an alkaline medium. The structure and the properties of graft copolymer are confirmed by Fourier transfer infrared spectroscopy (IR), X‐ray diffraction and thermogravimetric analysis (TGA). The mechanism is proposed to explain the generation of radicals and the initiation. The effects of reaction variables, such as the initiator concentration, ratio of 4VP to PA6, pH, as well as reaction temperature and time are investigated. Graft copolymers with high grafting efficiency (>95%) were obtained, which indicated that the DPC–PA6 redox system was an efficient initiator for this graft copolymerization. The quaternized PA6‐g‐P4VP (QPAVP) is proven to be an excellent adsorbent to heavy metal ions.     

Bi2Ti2O7薄膜的自组装法制备及表征

以Bi(NO₃)₃·5H₂O和Ti(OC₄H₉)₄为原料,采用自组装单层膜技术,在负载有功能化三氯十八烷基硅烷(octadecyl-trichloro-silane,OTS)的FTO基板上制备了Bi₂Ti₂O₇ 薄膜。基板表面的亲水性测试表明,紫外照射使OTS自组装单层膜表面由疏水转变为亲水,实现功能化。借助X射线衍射(XRD)、X射线能量色散谱(EDS)、扫描电子显微镜(SEM)和原子力显微镜(AFM)分析分别对Bi₂Ti₂O₇薄膜的组成、结构和微观形貌进行了表征。结果表明,沉积溶液浓度为0.02 mol·L^-1时,所得Bi₂Ti₂O₇薄膜均匀致密。560 ℃热处理1 h、厚度为0.4 μm的Bi₂Ti₂O₇薄膜在100 kHz的介电常数为153,介电损耗为0.089。     

Synthesis of Sub-100 nm Nanoparticles by Emulsifier-free Emulsion Polymerization of α-Methylstyrene,Methyl Methacrylate and Acrylic Acid

The emulsifier-free emulsion copolymerization of α-methylstyrene (AMS) and methyl methacrylate (MMA) in the presence of functional monomer acrylic acid (AA) was carried out in batch process, giving birth to sub-100 nm nanoparticles. The kinetics of polymerization was investigated. The morphology and size of particles were monitored by TEM. The influences of the functional monomer AA concentration, initiator ammonium persulfate (APS) concentration, and polymerization temperature were studied. It was found that AMS caused a drastic decrease in both the rate of polymerization and the average degree of polymerization. The activation energy calculated from Arrhenius plot turned out to be 83.6 kJ/mol.     

Electroless plating of copper on fly ash cenospheres using polyaniline‐Pd activation

The polyaniline of different intrinsic oxidation states, viz., the emeraldine (EM) and the leucoemeraldine (LM) states, were coated on 3‐aminopropyltriethoxy silane modified fly ash cenospheres. Without prior sensitization by SnCl₂ solution, Pd activation by PdCl₂ solution was carried out on EM and LM laden cenospheres, followed by electroless plating of copper (Cu). The topography and composition of the composites were characterized by scanning electron microscopy, X‐ray diffraction, and X‐ray photoelectron spectroscopy, etc. The results indicate that the oxidation state of the LM layer showed a much bigger increase than that of the EM layer in the Pd activation process, while coupled Pd reduction underwent to a more extent on the LM layer. The metallic Pd atoms on the LM and EM layers surface initiated the subsequent electroless plating of Cu, and the coated Cu on LM laden cenospheres had a much more uniform and compact morphology than that on EM laden cenospheres. Copyright © 2012 John Wiley & Sons, Ltd.     

Addition of Organometallic Reagents to Chiral N‐Methoxylactams: Enantioselective Syntheses of Pyrrolidines and Piperidines

Enantioselective iridium‐catalyzed allylic substitutions were used to prepare N‐allyl hydroxamic acid derivatives that were suitable for ring‐closing metathesis, giving N‐methoxylactams. Reactions of these derivatives with Grignard or organolithium compounds gave hemiaminals, which could be reduced diastereoselectively via acyliminium intermediates to give cis‐piperidines or cis‐pyrrolidines with substituents in the 2,6‐ or 2,5‐positions, respectively. In addition, compounds with a quaternary carbon center could be synthesized by corresponding reactions with potassium cyanide/AcOH. The procedures were applied in the syntheses of alkaloids (?)‐209D and (+)‐prosophylline.     

CuI‐Catalyzed Multicomponent Synthesis of Aminoindolizines from Aldehydes,Amines, and Alkynes under Solvent‐Free Conditions

A direct and efficient approach to 1‐aminoindolizines through three‐component one‐pot reaction of heteroaryl aldehydes, secondary amines and terminal alkynes catalyzed by CuI under solvent‐free conditions has been developed. This methodology provides a rapid access to substituted aminoindolizines with good yields (up to 97%).