2012, 29(7).
Abstract:The block copolymer of PSt-b-POEOMA-b-PSt with the end of -COOH functional group has been synthesized by reversible addition fragmentation chain-transfer (RAFT) using S,S′-Bis(α,α′-dimethyl-α-acetic acid)-trithiocarbonate (BDATC) as the chain transfer agent. The block copolymer containing hydrophilic end groups can be assembled into the core-shell nanoparticles for drug-loaded polymer template. The architecture of the copolymer was confirmed by FTIR, 1H NMR spectra and GPC. Furthermore, through the thermogravimetric (TG) and differential scanning calorimetry calorimeter (DSC) methods, the thermal properties of the three different proportions of block copolymers were studied. Results showed that RAFT polymerization was successful to synthesize the designed block copolymer; the molecular weight distribution of the controlled block copolymer was about 1.35. And the block copolymers had good thermal stability; the compatibility of the two components could be speculated by the change of the glass transition temperature (Tg).
ZHANG Wei-min , SUN Li , FAN Gao-chao , HONG Fang , FENG Yu , SU Zhi-Xing
2012, 29(7).
Abstract:A new 1,4-diketopyrrolo[3,4-c]pyrrole(DPP)-based molecule (I) was designed and successfully synthesized with 2,2'-bithiophene as starting material via bromination, selective debromination, amination, alkylation, cyanation,condensation etc., and the product and precursors were confirmed by 1H NMR, 13C NMR, IR, MS and elemental analysis.Compound (I) shows good solubility in organic solvents, and an intense absorption between 530-700 nm.
2012, 29(7).
Abstract:In this study, gelatin-gum arabic nanocapsules containing the two-phase core materials were prepared by complex coacervation, in which the TiO2 nanoparticles modified with stearic acid and dispersed in Tetrachloroethylene(TCE)were encapsulated. The effects of various microencapsulation parameters were also experimentally investigated. The obtained materials were characterized by scan electron microscopy (SEM) and transmission electron microscopy (TEM). The results indicated that the surface of the nanocapsules is smooth and clear. the two-phase dispersion was encapsulated in nanocapsules and the diameter of TiO2 nanoparticles was ~50 nm. The resulting nanocapsules have 0.96 μm in average diameter with a wall thickness of ~18 nm.
CUI Yan-li , HUANG Yan , ZHANG Qi
2012, 29(7).
Abstract:An isatin Schiff base derivative, 3-((2-hydroxynaphthyl)methyl)hydrazono- indilin-2-one(HNHI) was designed and synthesized. Its structure was characterized by 1H NMR、13C NMR and element analysis. The influences of different metal ions on its UV-Vis absorbtion spectra and fluorescence spectrum were studied. The results showed that the absorption spectra of HNHI had good response to Cu2 , Co2 and Ni2 , and appeard a new peak in the long wavelength region. Then the solution was turned to pink from colorless. Besides, the fluorescence spectrum of HNHI had good selectivity to Cu2 , Co2 and Ni2 with obvious fluorescence enhancement.
2012, 29(7).
Abstract:Reacted of gramine remification 2-benzoisothiazolin-3-one (BIT) with Copper acetate and Zinc acetate obtained two organic/inorganic complexes: [Zn(BIT-H)2] (1), [Cu(BIT)(BIT-H)(CH3COO)] (2). the structures of the complexes were characterized by EA, IR, 1H NMR and UV-Vis, Antibacterial experiments of the two complexes were studied, The MIC of the two complexes with Escherichia coli : 2.344?0-3 mg/mL, 1.172?0-3 mg/mL. The MIC of the two complexes with Staphylococcus aureus: 1.172?0-3 mg/mL, 1.172?0-3 mg/mL.
2012, 29(7).
Abstract:Preparation of β-cyclodextrin/vanillin microcapsules through spray-drying method has been investigated by evaluation of loading efficiency and loading rate of the microcapsules. The optimal production conditions are as follows: ρ(β-cyclodextrin)= 79.5g?L-1, n (vanillin)∶n (β-cyclodextrin) = 0.8∶1.0, V (anhydrous ethanol)∶V (water) = 1∶10, inlet temperature =130 癈, drying air speed= 3.9 m?s-1, flow rate= 15 mL?min-1. Loading efficiency and loading rate of the product were 69.1% and 10.6 %, respectively. FTIR spectra were used to prove intermolecular interaction between vanillin and β-cyclodextrin. TG-DSC results confirmed the thermal stability of vanillin was improved after encapsulating by β-cyclodextrin. The particle size analysis suggested that variation value of the average particle sizes of β-cyclodextrin was in the range of 0.14μm ~ 1.2μm and that of product was in the range of 0.011μm ~ 0.22μm during 50 days storage, the latter was much smaller than the former, which further certificated the fabrication of supramolecular microcapsules.
2012, 29(7).
Abstract:Abstract:A new type of (AB)n polyether-block-polysiloxane (PBMS) was synthesized by hydrosilylation reaction between Si-H terminated polydimethylsiloxane and allyl- polyoxyethylene-polyoxypropylene (AAF) in the presence of H2PtCl6-isopropyl alcohol. And its chemical structure was characterized by FT-IR spectroscopy. The defoaming agent emulsion was formulated from polydimethylsiloxane, hydrophobic silicon dioxide, MQ silicone resin, the PBMS and so on. Starting from preparation of silicone defoaming surfactant, conditions that affect the defoaming and inhibiting performance, such as mass fraction of these defoaming surfactants, PBSO with different structures, the length of silicon chain and molecular weight of AAF polyether, were investigated. Experiment results showed that the defoaming agent can rapidly broke down 100mL bubble in 7.8″, with bubble-restrain time of 45.8′, and no delamination, no emulsion breaking under the base condition(pH =12) and at high temperature(65°C) for 24h.
2012, 29(7).
Abstract:A practical method for the racemization of L-arginine and an enzymatic method for optical resolution of DL-arginine by L-arginine amidinase have been developed. We obtained D-arginine and L-ornithine hydrochloride after isolation and purification. Many factors affected the racemization and enzymatic reaction. The whole process of racemization by this method can be completed within 2.5 h. The ratio of the racemization was as high as 74.5%. The result shows that the optimum conditions of enzymatic reaction were: 35 ℃, pH=10, c( DL-arginine) = 40 g/L and c(L-arginine amidinase) = 0.2 g/L. The conversion rate of L-arginine was higher than 98%. The products were separated and purified on ion-exchange resin. The optical purity of products were 99%.
2012, 29(7).
Abstract:With Gonocaryum lobbianum (Merr.) Kurz fruits as the raw material, the Gonocaryum lobbianum (Merr.) Kurz fruit oil were extracted by microwave-assisted extraction and supercritical CO2 fluid extraction, the chemical composition and relative content of each fatty acid of the oils by methyl esterifying using alkali catalyst and BF3-MeOH catalyst were identified by GC-MS. There was no significant difference of the chemical composition of the oils in these two extractions. A difference was methyl esterifying by alkali catalyst had identified seven kinds of fatty acids, whereas methyl esterifying by BF3-MeOH catalyst had identified ten. In the following four methyl esterifying ways: MAE(alkali catalyst), SFE-CO2(alkali catalyst), MAE(BF3-MeOH catalyst),SFE-CO2(BF3-MeOH catalyst), the highest content of fatty acids was octadecenoic acid (69.44%, 69.04%, 64.92%, 64.69%) , followed by hexadecanoic acid (20.82%, 21.01%, 21.69%, 21.45%), then octadecadienoic acid (6.33%, 6.03%, 6.33%, 6.13%). The total content of unsaturated fatty acids was 76.75%, 75.91%, 74.77% and 74.30% respectively.
2012, 29(7).
Abstract:On the basis of the stability constant determination of zingiberene-Ag+ coordination compound, zingiberene static adsorption on silver nitrate modified silica gel was compared with that on silica gel , and the thin layer chromatography of Ginger oleoresin on argentated silica gel G pre-coated plate with that on silica gel G pre-coated plate, finally modified silica gel column chromatography was used to isolate zingiberene from ginger oleoresin.The comparison results indicated that zingiberene static adsorption was weak when silica gel was treated as medium, and the adsorption capacity was enhanced after silica gel was modified with silver nitrate, whenever the adsorption conforms to the Langmuir monomolecular adsorption. Zingiberene-Ag+ π coordination compound could be formed with the stability constant was 1.46×10-2L•mol-1when silver nitrate was added.The stability of sesquiterpene-Ag+ coordination compounds is related to their structure and the solvents, consequently when silica gel was modified with silver nitrate, the selective adsorption of zingiberene was increased, zingiberene was effectively separated from Ginger oleoresin and the purity of the final products was 97.22% with 87.15% recovery.
WANG Da-hong , YUAN Jiang-feng , GONG Qiang
2012, 29(7).
Abstract:Nine macroporous resins with different polarities were evaluated for the static adsorption of quinoxalone. Adsorption kinetics curves and adsorption isotherm of quinoxalone were studied at 25℃ and the process of adsorption was simulated with Langmuir and Freundlich equations. The results showed that XAD16 and HPD-100 resins displayed higher adsorption and desorption performance for quinoxalone than the other resins. Their adsorption capacity and desorption ratio were higher than 600 μg/g dry resin and 70%, respectively. Comparing the correlation coefficient of Langmuir and Freundlich equation, .the former were 0.9726 and 0.9871,respectively; the latter were 0.8879 and 0.9412, respectively。So, D101 was the better and the adsorption capacity arrived to 976 μg per gram dry resin. It was concluded that D101 resin was the ideal macroporous resin for the adsorption of quinoxalone from the fermentation broth of myxobacteria Stigmatella WXNXJ-B.
2012, 29(7):0-0.
Abstract:The carbon supported Pd (Pd/C) catalyst was prepared with complex reduction method by sodium borohydride and ethylene glycol, respectively. The transmission electron microscopy (TEM) and X-ray diffraction (XRD) spectrum characterizations indicate that Pd nanoparticles of the Pd/C catalyst prepared by ethylene glycol have a smaller particle size, uniform particle size distribution and higher relative crystalinity. The average size and relative crystalinity of the Pd nanoparticles are as small as 4.2±2 nm and 1.88, respectively. The electrochemical measurements demonstrate that the electrocatalytic activity and stability of the Pd/C catalyst prepared by ethylene glycol for formic acid oxidation are better than that of the Pd/C catalyst prepared by sodium borohydride.
2012, 29(7).
Abstract:3-(1H-pyrrole-2-carbonyl)propionic acids (2a ~ 2c) were synthesized, in yields of 84.7 % ~ 91.2 %, by alkylations of methyl 3-(1H-pyrrole-2-carbonyl)aminopropionate (3) with alkyl halides and followed by hydrolyzation; the title compounds, 1a ~ 1c, were obtained via cyclizations of the acids (2a ~ 2c) in the presence of polyphosphoric acid and diphosphorus pentoxide, in yields of 69.1 % ~ 77.2 %. The overall yields of the three step reactions were 61.8 % ~ 69.1 %. And the α-glucosidase inhibitions of the three title compounds have also been studied.
强涛涛 , ZHANG Guo-guo , LUO Min , WANG Xue-chuan
2012, 29(7):0-0.
Abstract:A series of hyperbranched poly(amine-ester) with terminal alcohol group(HPAE-OH) were synthesized by the polycondensation of N,N-diethylol-3-amine-methylpropionate [prepared by the Michael addition reaction of methyl acrylate(MA) with diethanolamine(DEA)] as an AB2-type monomer with trimethylol propane(TMP) as the core moiety, proceeding in one-step procedure in the melt with p-toluenesulfonic acid(p-TSA) as catalyst. Then, it was modified by maleic anhydride to obtain hyperbranched polymer with terminal carboxyl group (HPAE-C). The appropriate reaction conditions were optimized: catalyst do sage 0.7%, molar freed ratio n(OH) ∶n(maleic anhydride) =1∶1.1, reaction time 4h and temperature 80℃. The obtained polymers were characterized by IR、1H-NMR and 13C-NMR, the surface activity of polymer was investigated by Surface Tension.
2012, 29(7).
Abstract:PVP/ZnO-TiO2 composite nanofibers were fabricated through a combination of sol–gel and electrospinning methods using polyvinglpyrrolidone ( PVP) as starting materials. ZnO-TiO2 nanofibers of 100–200 nm diameter were obtained by high temperature calcinations of the inorganic organic PVP/ZnO-TiO2 composite fibers.The materials were characterized by DSC- TGA, FT-IR and SEM. The process of the photocatalytic degradation of methylene blue using ZnO-TiO2 nanofiber as catalyst was investigated. The results show that the ZnO-TiO2 nanofiber dopped 3% ZnO has the highest photocatalytic activity for methylene blue degradation, the degradation rate of methylene blue solution reached 99% under sunshine for 6 h., and it’s still 95% after eight times reuse.
2012, 29(7).
Abstract:A graft copolymer of guar gum with acryl amide was made by using ammonium ceric nitrate/nitric acid as initiator. The effects of AM/GG, initiator concentration, reaction temperature and reaction time on polymerization were investigated. The results indicated that: The grafting ratio and comonomer conversion of grafting copolymerization were 147.05% and 87.7% when AM/GG=3:2, initiator concentration was 4mmol/L, reaction time was 4h and reaction temperature was 45℃. The largest molecular of graft copolymer could reach to 1.73x106. The analysis of IR spectrum and SEM turned out that AM did graft to the molecular chain of guar gum.TGA indicated that graft AM has no effect on the thermal stability of guar gum.
2012, 29(7).
Abstract:With cyanuric chloride as the crosslinking monomer and 4,4′-diamino stilbene-2,2′-disulfonic acid (DSD acid) as raw materials, a new yellowing inhibitor for high-yield pulp was synthesized through joining the ultraviolet absorber 2,4-dihydroxy-benzophenone and triazine-stilbene fluorescent brighteners in the same molecule by the size of nucleophilicity method. The new product had the function of fluorescent whitening and absorbing ultraviolet. Its structure was demonstrated by FT-IR besides the physical properties were examined by UV-vis and photoluminescence(PL) spectra and the effect of anti-yellowing were evaluated – as the surface sizing agent on handsheet of chemimechanical pulps by using the ultraviolet aging apparatus. The results showed that the best dosage of the new yellowing inhibitor was 1.0% and could be proposed as a applicable yellowing inhibitior for lignin-content paper products, besides the brightness atbilities of chemimechanical pulp handsheets were increased more by application of the new yellowing inhibitor as surface sizing agent than those does by application of fluorescent brighteners and ultraviolet absorber alone respectively and declining brightness of hand-sheets treated by new yellowing inhibitor was 1.36%ISO and 4.25 %ISO less than hand-sheets treated by them after 48h UV accelerated irradiation..
2012, 29(7):0-0.
Abstract:With the increasing demand of using cellulose more effectively, modification of cellulose by graft polymerization provides a significant route to combine the advantages of natural and synthetic macromolecules for a wide range of potential applications. Synthesis of cellulose-graft-PHEMA copolymer via homogeneous atom transfer radical polymerization (ATRP) in the ionic liquid was researched in this article. FTIR, 1H NMR and GPC were carried out to analyze the effects of different solvents on the polymerization conditions, grafting efficiency, molecular weight distribution, thermal stability and the changes in shape in different solvents of the copolymer as well. The results indicated that the grafting efficiency increased with the increase of reaction time. The obtained graft copolymer cellulose-graft-PHEMA showed good thermal stability, and the copolymer could aggregate into spherical particles with 50nm diameter in DMF and 100nm diameter in the selective solvent butanone.
2012, 29(7).
Abstract:A new method for the determination of volatile organic compounds (methanol, acetone, methyl acetate, tertiary butanol, vinyl acetate and ethyl acetate) in adhesive for cigarette by headspace gas chromatography was investigated. The effects of temperature programming, equilibrium time, equilibrium temperature and quantity of the adhesive on the experimental result were discussed, and an optimal process variable for the determination of volatile organic compounds was obtained. The results show that the linearity range of this method is 0~400礸 for methyl alcohol, 0~40礸 for acetone, 0~92礸 for methyl acetate, 0~75礸 for tertiary butanol, 0~75礸 for vinyl acetate and 0~45礸 for ethyl acetate, respectively. The relative standard deviations was 0.6%~2.7%, and the recovery was 90.8%~104.2%. This method to determiante volatile organic compounds in adhesive for cigarette is simple, rapid, accurate.
2012, 29(7).
Abstract:This paper is research on Hofmann degradation to prepare polyvinylamine (PVAm) . Material ratio, reaction temperature, addition mode and other reaction conditions which have effect on amination degrees were discussed as well as recycle of the mixed solution containing alcohol and base. Results show that the amination degrees of product is 84.54% by using Commercial nonionic polyacrylamide (PAM) , the base solution recycling from the mixture can be used 3 times. In this modified Hofmann degradation,polyacrylamide was added into NaClO and NaOH solution direactly to make chloro- polyacrylamide, then put it into base solution,in order to increase yield per volume solution.
2012, 29(7).
Abstract:4,4′-ether dinaphthalene 1,1′,8,8′-tetracarboxylic dianhydride was synthesized by using acenaphthene as raw material through Nitration, reduction, Bucherer reverse reaction, etherification and oxidation. The conditions of phenol self-coupling etherification under microwave irradiation were investigated. Results showed that the best conditions under microwave irradiation were the power of 600 W, the temperature of 150 ℃, and the reaction time of only 2 h , with the yield of 57.8%.
HU Tian-jing , HU Bing-cheng , XU Shi-chao , HUANG Xiu-you
2012, 29(7).
Abstract:[2,7,12,18-tetramethyl-3,8-bis(-2-hydroxy ethyl)-13,17-methoxy carb- onyl ethyl]-porphyrin was prepared from hemin by a three-steps reaction including demetalation, esterification, anti-Markovnikov addition. In the synthesis process of protoporphyrin dimethyl ester, environmental friendly ultrasound method was put to use with the yield of 91.6%. [2,7,12,18- tetramethyl-3,8-bis(-2-hydroxy ethyl)-13,17-methoxy carbonyl ethyl]-porphyrin was obtained from the anti-Markovnikov addition of protoporphyrin dimethyl ester with BH3-THF with the yield of 64.3% under reasonably optimized conditions. The target products were characterized with 1HNMR, MS, UV-vis and IR.