新型甘露醇基凝油剂的制备及性能研究

通过甘露醇和环己酮的缩酮反应,合成了具有相选择性的新型糖基凝油剂-环己酮缩甘露醇。考察了反应时间、催化剂用量、分子筛用量、底物配比等多个因素对产物产率的影响。结果表明,分子筛用量为12g、催化剂用量为0.8g、环己酮与甘露醇摩尔比为6.2∶1的条件下反应1h,产率为52%。对所制备的环己酮缩甘露醇的凝油能力测试表明,它可以凝固汽油、硅油等多种油类,柴油、汽油和硅油凝固的最小浓度分别为0.74(wt)%、2.70(wt)%和0.39(wt)%。     

Preparation and thermal properties of a novel flame-retardant coating

A novel silicone and phosphate modified acrylate (DGTH) was synthesized and characterized by ¹H NMR and FTIR. It was found that DGTH could be cured both by UV radiation and moisture mode with FTIR. The flammability and thermal behavior of the cured film were studied by the limited oxygen index (LOI), thermogravimetric analysis (TG) and real time Fourier transform infrared (RT-FTIR). The LOI value of the cured film is 48 and the TG data shows that the cured film has three characteristic degradation temperature regions, attributing to the decomposition of phosphate and polyurethane to alcohols and isocyanates, thermal pyrolysis of alkyl chains, and decomposition of unstable structures in char, respectively. The RT-FTIR data implies that the degraded products of phosphate form poly(phosphoric acid) further catalyse the breakage of carbonyl groups to form an intumescent char, preventing the samples from further burning.     

Preparation,properties and reactivities of novel platinum compounds containing a thiomethoxymethyl group

Oxidative addition of ClCH₂SCH₃ to PtL₄ afforded trans-PtL₂(CH₂SCH₃)Cl (Ia, L = Ph₃P;Ib, L = MePh₂P). Treatment of I with NH₄PF₆ or Et₃OBF₄ in CH₂C1₂ gave ionic species, [PtL₂(CH₂SCH₃)]X (II, L = Ph₃P, MePh₂P, X = BF₄, PF₆), while similar treatment with MeSO₃F in benzene yielded a new type of stable dimethylsulfonium methylide—platinum complex, trans-[PtL₂(CH₂SMe₂)Cl] SO₃F (IIIa, L = Ph₃P; IIIb, L = MePh₂P). Action of H₂O₂ on Ia gave [Pt(Ph₃P)(μ-CH₂SCH₃)C1]₂ (IV) and its triphenylarsine analog, [Pt(Ph₃As)(μ-CH₂SCH₃)C1]₂ (V) was prepared in one step by oxidative addition of ClCH₂SCH₃ to Pt(AsPh₃)₄. The structural difference between [Pt(Ph₃P)(μ-CH₂SCH₃)C1]₂ and Pd(Ph₃P)- (CH₂SCH₃)C1 is discussed in terms of the difference in the ionization potential from d¹⁰ to d⁸ electronic state of metals.     

Preparation and properties of novel polyhydrazides

A new class of polyhydrazides having aromatic as well as aliphatic units has been synthesized by low-temperature solution polycondensation from equimolar amounts of diacid chloride and dihydrazides in HMPT as solvent. These polyhydrazides have poor solubilities and their intrisnsic viscosities ranged from 0.2 to 0.6 dl/g. X-ray diffractograms of these polyhydrazides show that the polymers having terephthalic acid dihydrazide unit were more crystalline and all the polymers have densities in the range of 1.2-1.8 g/cm³. Thermogravimetric analysis of these polyhydrazides showed initial weight losses commencing at 220–300°C in both air and nitrogen.     

Preparation, characterization, and FET properties of novel dicyanopyrazinoquinoxaline derivatives

[structure: see text] A series of the title dicyanopyrazinoquinoxaline derivatives have been prepared and characterized by using single-crystal X-ray structure analysis and redox potential measurements. They have strong electron-accepting properties due to the pyrazinopyrazine skeletons as well as the cyano groups. Substituents can be easily introduced at the benzene ring and control the HOMO-LUMO energy gap and the molecular packing. They show clear n-type transistor properties in the FET devices.     

Preparation,properties, and antibacterial behavior of a novel cellulose derivative containing lactam groups

Lactam groups were introduced onto the backbone of hydroxyethyl cellulose (HEC) to modify properties, such as solubility in organic solvents and solution viscosity and to introduce possible antibacterial activity. Functionalization was achieved using 1‐(hydroxymethyl)‐2‐pyrrolidinone (HMP), and the functionalization reactions were investigated using NMR spectroscopy. The covalent attachment between HEC and HMP was confirmed using ¹H‐¹³C correlated NMR experiments. Degrees of functionalization were calculated using integrated ¹³C NMR spectra, with values of up to 0.9 being demonstrated on the primary alcohol functionality of HEC. The functionalized HECs showed markedly different properties to unfunctionalized HEC, including the ability to swell considerably in water. Functionalized HEC displayed increased thermal stability and reduced solution viscosity compared with unfunctionalized HEC. Moreover, functionalization altered the bacterial adhesion characteristics compared with unfunctionalized HEC. © 2014 The Authors. Journal of Polymer Science Part A: Polymer Chemistry Published by Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2015 , 53, 68–78     

Preparation and thermal properties of a novel flame retardant copolymer

A monomer, acryloxyethyl phenoxy phosphorodiethyl amidate (AEPPA), was synthesized and characterized using Fourier transform infrared (FTIR), ¹H nuclear magnetic resonance spectroscopy (¹H NMR) and ³¹P NMR. The copolymer with various amounts of styrene (St) was obtained by the free radical bulk polymerization between AEPPA and St, and characterized using ¹H NMR. The thermal properties of the copolymers were investigated with thermogravimetric analysis (TGA) in air and nitrogen atmosphere, and differential scanning calorimetry (DSC). The TGA results in air indicated the copolymers with AEPPA show higher thermal stability than those without AEPPA. However, the TGA results in nitrogen showed that the decomposition temperature decreased and the char residue increased with the increase of AEPPA. The glass transition temperature (T_g) of the copolymers from DSC indicated that a inverse proportion was observed between T_g and the amount of AEPPA incorporated. The flammability of the copolymers was evaluated by microscale combustion calorimeter (MCC). The MCC results showed that AEPPA can decrease the peak heat release rate (PHRR) and the heat release capacity (HRC), and the sample CP10 shows the lowest PHRR and HRC.     

Preparation and novel reduction reactions of vinamidinium salts.

Substituted acetic acids and formamides react in the presence of phosphorus oxychloride to yield the vinamidinium hexafluorophosphate salts 5a-d, 6a-d, and 7 in moderate to good unoptimized recrystallized yields (40-67%) as easily handled nonhygroscopic solids. The 1,3-differentially substituted vinamidinium salts 8 was prepared by amine exchange in 81% yield as are the cyclic diazapinium salts 9 and 10 in > 76% yield. The symmetrical 2-chlorovinamidinium 11 was prepared by displacement of 3 in 71% yield. The 2-chlorovinamidinium salts are cleanly reduced to the parent vinamidinium salts 12-16 using HI or PPh3/pTSA in up to 99% assay yield.     

Preparation,rheological and drag reduction properties of hydrophobically associating polyacrylamide polymer

Hydrophobically associating polymer (HAMDP) was synthesized by using acrylamide, acrylic acid, 2-acrylamido-2-methylpropane sulfonic acid and dodecyl 2-methylacrylate as main monomers. Dynamic rheometer and self-made simulation evaluation apparatus were used to test the rheological and drag reduction properties of HAMDP. With the mass concentration increased, the apparent viscosity of HAMDP increased. The critical aggregation concentration was 2.29g/L. With the changement of the strain, the elastic modulus was larger than viscous modulus. With the increment of HAMDP, the area of thixotropic loop increased. Compared with commercial polyacrylamide, the drag reduction rate of HAMDP could be up to 62.38%.     

Preparation and properties of novel palladium compounds containing a thiomethoxymethyl group

Oxidative addition of chloromethyl methyl sulfide to Pd(Ph₃P)₄ provided a good yield of Pd(Ph₃P)₂(CH₂SCH₃)Cl (I) whose ¹H NMR and molecular weight data showed that dissociation of either the phosphine or the chloride ligand occurs in CH₂Cl₂ solution. In accord with such equilibria, repeated crystallization of I from CH₂Cl₂ and Et₂O gradually removed the triphenylphosphine set free in these solvents to give the monomeric complex. Pd(Ph₃P)(CH₂SCH₃)Cl (III), while treatment of 1 with NH₄PF₆ in CH₂Cl₂ and acetone gave the cationic complex [Pd(Ph₃P)₂(CH₂SCH₃]PF₆ (II),¹H NMR spectra of II and III are discussed in terms of a three-membered chelate structure arising from coordination of sulfur with palladium     

Preparation and expansion properties of a novel UV-curable intumescent flame-retardant coating

Journal of Thermal Analysis and Calorimetry - N,N′-bis(2,4-di(acryloyloxyethyl)-[1,3,5]-triazin-2-yl)-hexane-1,6-diamine(BDAETH) and 2,2-dimethyl-1,3-propanediol glycerol-methacrylate...     

Preparation, properties, and reduction of heteroaromatic quinoids with 1,4-diazacyclopentadien-2-ylidene terminals

New n-type heteroaromatic quinoids with 1,4-diazacyclopentadien-2-ylidene terminals were prepared. These quinoids possess strong electron-accepting properties, comparable to dicyanomethylene analogues. Both the radical anions and dianions were generated by metal reduction using 3% Na-Hg in THF and were spectroscopically characterized.     

Preparation, properties, and synthetic potentials of novel boronates in a fluorous version (fluorous boronates)

[reaction: see text] A series of boronic acids were attached to a fluorous tag by esterification. Functional transformations of these boronates together with the fluorous Suzuki coupling reaction illustrated their usefulness in fluorous-phase techniques.     

Preparation,characterization, antioxidant properties of novel Schiff bases including 5-chloroisatin-thiocarbohydrazone

Research on Chemical Intermediates - Thanks to its pharmaceutical properties, the Schiff group of isatin has recently had a wide range of uses. In this study, seven new Schiff bases of isatin and...     

Preparation, photo- and electro-luminescent properties of a novel complex of Tb (III) with a tripod ligand

A novel Tb(III) complex TbL (L=tris[2-(2-carboxyphenoxy)ethyl]amine, H3L) was synthesized and characterized by means of elemental analyses, IR spectra, thermal analyses, and molar conductivity measurement. The photoluminescent properties of the complex were investigated. In addition, PVK doping Tb(III) complex was fabricated as the emissive layer by spin-coating and its electroluminescent properties were studied, in which the structure of the device was ITO (indium tin oxide)/PVK (polyvinylcarbazole)/PVK: TbL/PBD (2-(4-biphenylyl)-5-(4-tert-butylphenyl)-1,3,4-oxadiazole)/LiF/Al. It was indicated that pure green and narrow bandwidth emission at 545nm from photoluminescence of TbL complex film and the organic electroluminescent device is the characteristic emission of Tb(III) ion, and the electroluminescence spectrum of the device was very similar to that of the photoluminescence of TbL complex film. The lowest triplet level of the ligand was calculated from the phosphorescence spectrum of GdL in N,N-dimethyl formamide (DMF) dilute solution determined at 77K, and the energy transfer mechanisms in TbL complex were discussed.     

Preparation and characterization of a novel stimuli-responsive nanocomposite hydrogel with improved mechanical properties

A novel stimuli-responsive organic/inorganic nanocomposite hydrogel (NC hydrogel) with excellent mechanical properties was synthesized by in situ polymerization of 2-(2-methoxyethoxy) ethyl methacrylate (MEO(2)MA), oligo (ethylene glycol) methacrylate (OEGMA) and acrylic acid (AAc), as the polymeric matrix (PMOA), and fibrillar attpulgite (AT), as the reinforcer and cross-linker. The effect of the AT content on the mechanical properties for the swollen and dried NC hydrogels was determined by tensile testing and dynamic mechanical analysis (DMA), respectively. The tensile testing results showed that the incorporation of AT nanoparticles significantly enhanced the mechanical properties of NC hydrogels. As the content of AT increased, the tensile strength, tensile modulus and effective cross-linked chain density increased. The DMA results showed that the storage modulus of AT/PMOA NC hydrogels was increased and the glass transition temperatures shifted to higher temperature compared to the pure PMOA hydrogel, which further indicated that the enhancement of mechanical property depended upon the presence and content of AT. In addition, the faster swelling rates of the NC hydrogels were observed in comparison with the corresponding physically cross-linked PMOA hydrogel, except for 1% AT/PMOA sample. However, the deswelling kinetics of NC hydrogels was obviously retarded.     

Preparation,characterization, and application of a novel immobilized carboxypeptidase B

Pig pancreas carboxypeptidase B has been immobilized by covalent attachment to a polyacrylamide-type bead support possessing carboxylic functional groups activated by water-soluble carbodiimide. The optimum conditions of immobilization were determined. The activation of the support and the coupling reaction were performed in 0.1 M sodium citrate/sodium phosphate buffer (pH 4.5) using a support-carbodiimide-enzyme weight ratio 4:8:1 at 0-4 degrees C. Under such conditions, the highest activity achieved was 6700 U/g solid. The catalytic properties and stability of immobilized carboxypeptidase B were studied and compared with the corresponding properties of the soluble enzyme. The specific activity of the immobilized enzyme calculated on bound protein basis was about 70% of that of soluble enzyme. The optimum pH for the catalytic activity of the immobilized carboxypeptidase B was practically identical with that of soluble enzyme (pH 7.6-7.7). The apparent optimum temperature of the immobilized carboxypeptidase B was about 7 degrees C higher than that of the soluble enzyme. With hippuryl-L-arginine as substrate, Kmapp value of the immobilized enzyme was tenfold higher than the Km value of the soluble enzyme. The conformational stability of the enzyme was markedly enhanced by the strongly hydrophylic microenvironment in a wide temperature and pH range. The immobilized carboxypeptidase B was used for stepwise digestion of cytochrome C.     

Preparation and properties of novel benzoxazine and polybenzoxazine with maleimide groups

A benzoxazine compound with a maleimide group, 3‐phenyl‐3,4‐dihydro‐2H‐6‐(N‐maleimido)‐1,3‐benzoxazine (HPM‐Ba), was prepared from N‐(4‐hydroxyphenyl)maleimide, formaldehyde, and aniline. The chemical structure of HBM‐Ba was identified by FT‐IR, ¹H‐NMR, and elemental analysis. HPM‐Ba showed a melting point of 52–55 °C and good solubility in common organic solvents. HPM‐Ba showed a two‐stage process of thermal polymerization. The first stage arose from the polymerization of maleimide groups, and the second one was the ring‐opening reaction of benzoxazine groups. Fusible polymaleimides with a Tg of around 100 °C could be obtained by thermally polymerizing HPM‐Ba at 130 °C. Further polymerizing the polymaleimides at 240 °C resulted in a completely cured resin showing a Tg at 204 °C. Good thermal stability and self‐extinguishing behavior was observed with the cured polybenzoxazine resins. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 5954–5963, 2004