• Volume 32,Issue 5,2015 Table of Contents
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    • >Review and monographs
    • A Review of Sulfate Reducing Bacteria Inhibitor for Oilfield Wastewater of Water-Flooding

      2015, 32(5).

      Abstract (1094) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Sulfate reducing bacteria (SRB) is one of the main factors causing microbial corrosion and environment pollution in the oil field water injection system. SRB can lead to the corrosion of metal pipelines and equipment, and the corrosion product ferrous sulfide and ferrous hydroxide and bacteria itself can be packaged by oil parcel causing plugging of pipeline and formation. In addition, the polyacrylamide polymer can be degraded in the presence of SRB, consequently affecting the subsequent development of enhancing oil recovery. At present, the most common and effective method to inhibit SRB in oil field is the chemical method. In this paper, we summarized the commonly used SRB chemical inhibitor in water-flooding and according to the sterilization mechanism the inhibitor can be divided into two types: oxidation inhibitors and non-oxidation inhibitor. Due to the different formation and the production process, the different kinds of chemical inhibitors should be adopted for water injection. Therefore, reseaching the novel, high efficiency and environment friendly SRB inhibitors is important in the future work.

    • >Functional materials
    • Preparation of Activated Carbons from Oiltea Shell Promoted by Zinc Chloride in Vacuum

      2015, 32(5).

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      Abstract:Activated carbons were prepared through oiltea shell heat decomposition under vacuum condition using zinc chloride as activating reagent.The factors affecting the adsorption properties of activated carbons were studied, including the concentration of zinc chloride, system pressure, activation time and activation temperatures. Surface area and porosity characteristics were determined with the analysis of N2 adsorption-desorption isotherms. The functional groups on the surface were analyzed by FT-IR spectroscopy. Microstructure of the sample was examined with scanning electron microscopy. The results show that the optimized condition for the preparation of activated carbon is as follows: zinc chloride concentration of 60%,immerse ration of 1:3, system pressure of 50kPa, activation temperature of 450℃ and activation time of 1h.The iodine absorption value and methylene blue absorption value of the prepared activated carbon are 1120 mg•g-1 and 373.16mg•g-1, respectively.The surface area is 2023.15 m2•g-1and total porous volume is 2.34 cm3•g-1 with an average porous diameter of 4.63 nm. The activated carbons prepared under vacuum condition have good absorption performance.

    • Phenolic Resin Assisted Synthesis SiO2/TiO2 Mesoporous Microspheres and Photocatalytic Performance

      2015, 32(5).

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      Abstract:Abstract: Nano-SiO2 was used as the matrix synthesised by Stöber method. The phenolic resin and hexadecyl trimethyl ammonium bromide (CTAB) was introduced to prepared SiO2/TiO2 mesoporous composite microspheres. Then the crystal structure, morphology , structure of the materials had been characterized by XRD, SEM, EDS , BET, BJH and FI-IR. Rhodamine B, the target degradation products, was used to evaluate the photocatalytic performance of the samples.The characterization results showed that the SiO2/TiO2 mesoporous composite microspheres were composed of TiO2 and SiO2, about 300 nm in diameter. TiO2 nanometer thin layer was uniformly deposited on the surface of SiO2 with Si-O-Ti bonds existed; The specific surface area of SiO2/TiO2 mesoporous composite microspheres was about 92.3 m2/g , approximately 3 times as big compared with the P25. Photocatalytic evaluation showed that the degradation of Rhodamine B rate for SiO2/TiO2 mesoporous composite microspheres reached 98%, improving significantly compared with P25.

    • Synthesis and Characterization of Zinc-based Aerogel Using Citric Acid as Template

      2015, 32(5).

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      Abstract:In this study, we developed the ZnO aerogel through dispersed inorganic sol-gel method using citric acid as template, which employed the properties of high apparent specific surface areas. The monolithic ZnO aerogel is prepared successfully on the basis of the dispersed inorganic sol-gel method with ZnCl2 and citric acid via supercritical fluid drying. By adopting FESEM, HRTEM, XRD, FTIR and BET, we learn that the aerogel has a typical three-dimensional porous structure featuring high surface area (177m2/g). The morphology of aerogel was evaluated by field-emmision scanning electron microscope (FESEM) and high-resolution transmission electron microscope (HRTEM), which suggest that the aerogel was made up of 3-D networks and the skeletal was composed of zinc oxide colloidal particles with amorphous carbon. The N2 adsorption/desorption shows that the aerogel has high BET surface area of 177 m?g, average pore diameter about 10-60nm, which means the aerogel possesses the typical characteristic of mesopore.

    • Studies on synthesis and photocatalytic properties of NiO-Ag2S nanocomposite

      2015, 32(5).

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      Abstract:NiO-Ag2S nanocomposite is synthesized by hydrothermal method with special photocatalytic. Combined the photocatalytic properties of both lamellarstructure NiO and Ag2S nannoparticles, the space of NiO are filled with Ag2S nannoparticles uniformly. Through the SEM, two-dimension EDX, and XRD analysis, the morphology and uniformity crystallinity of NiO-Ag2S nanocomposites are revealed. As a simulation reaction, the photocatalytic degradation of methyl orange in NiO-Ag2S nanocomposite suspension irradiated by 500 W Xe lamp isinvestigated. As a result, The photocatalytic ability of NiO-Ag2S nanocomposite is higher than NiO2 and Ag2S. And the photocatalytic efficiency is 30% higher than the physical mixture of NiO2 and Ag2S(mass ratio:1:1) after irradiating 180 min. We believe that p-n junction of NiO-Ag2S nanocomposite is the important factor for the high catalytic performance.

    • >Surfactants
    • The Synthesis of an Novel quaternary ammonium Cationic Surfactant and Its Solution Properties

      2015, 32(5).

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      Abstract:A novel quaternary ammonium cationic surfactant (N-octadecyl-N, N’-dimethyl-ethane-1, 2-diamine, C18DEDAM) was synthesized by 2-Chloroethylamine hydrochloride and Octadecyl dimethyl amine (C18DAM) at 70oC for 7h under the condition that the pH value was 7, and the compound structure was confirmed by IR and 1HNMR. The cmc was measured by conductivity measurement, and the cmc value is 4.6?0-3mol/L. C18DEDAM can form wormlike micelles as the NaSal concentration is 1 wt%. The shearing test shows that C18DEDAM-NaSal system has the shearing thinning ability that is the characteristic of wormlike micelles, and the viscoelastic test indicates that the system shows the characteristic of gel. Besides the surfactant can achieve high viscosity in acid condition, which indicate it is one kind of smart viscoelastic surfactant.

    • Synthesis and Surface Properties of Amphiphilic Linear-dendritic Carbosilane Block Copolymers

      2015, 32(5).

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      Abstract:Based on allylation of hydroxyl-terminated PEG and hydrosilylation of the allylic double bonds, two kind of linear-dendritic amphiphilic block copolymers with carbosilane hydrophobic head groups attached to PEG hydrophilic bridging chain were synthesized. The molecular structures of the copolymers were characterized with NMR and FTIR, and their surface properties were evaluated. The two copolymers showed good surface activities, and the CAC values are 5.13?0-4 and 4.83?0-5 mol?L-1,γCAC values are 32.48 and 32.21 mN?m-1 respectively. Moreover, two breaks were observed in the surface tension vs concentration curve for the two copolymers, which is believed to originate from rearrangement of the copolymer molecules on the air/water surface, and the molecular architecture of the copolymers at the surface layer were effected by the PEG segments and carbosilane branched blocks of the copolymers.

    • Physicochemical Properties and Phase Behavior of Mixed Systems Containing Glycoside-Based surfactant and Didecyldimethylammonium Chloride

      2015, 32(5).

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      Abstract:The properties and phase behavior of different glycoside-based surfactant/ didecyldimethylammonium Chloride (DDAC) mixtures have been investigated. The three glycoside-based surfactants are decyl glycoside (APG), dodecyl ethoxy glycoside (AEG) and disodium dodecyl ethoxy glycoside citrate (AEG-EC). For APG/DDAC, synergism was observed in surface tension, foaming and emulsifying properties, not in wetting ability. For AEG/DDAC, synergism was observed in foaming and emulsifying properties, while the wetting ability exhibited no such effect. The surface tension and wetting ability of AEG-EC/DDAC mixed systems showed synergism, while the foaming property not. Phase behavior of the glycoside-based surfactant/DDAC/water ternary system has also been carried out by polarized optical microscope. The phase diagrams are characterized by a micellar phase, a region of coexistence of lamellar and micellar phases and a lamellar phase.

    • Application of Polymerizable Cationic Fluorosurfactants in the Emulsion Polymerization of Fluorinated acrylate

      2015, 32(5).

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      Abstract:Fluorinated polyacrylate emulsion was synthesized via miniemulsion polymerization based on N-(perfluoro-octyl acetate, ethyl)-N-(ethanol acrylate) dimethyl ammonium bromide (PF8DM) as polymerizable cationic surfactant. The effect of the PF8DM content on the conversion rate of monomer and coagulum content was investigated; the impact of the PF8DM content on the emulsion stability and the film surface properties was studied. A comparative study of the surface properties of latex films prepared respectively by PF8DM and cetyltrimethylammonium bromideas as emulsifier was carried out. The results show that the monomer conversion rate is 95% and the gel rate is 0.6% when PF8DM content is 4 wt%. The as-prepared emulsion has excellent storage, dilution and centrifugal stability. The water contact angle of latex film is 118.6°when PF8DM content is 6 wt% . The latex film has low water absorption and excellent water repellent properties as the bonding rate of PF8DM reaches 89.4%. Under the same condition of the total fluorine content, the water absorption of latex film was greatly reduced and its hydrophobicity was enhanced significantly.

    • >Catalysis,separation and purification technology
    • Catalytic synthesis of C16 Guerbet alcohol by using supported CuO-NiO catalyst

      2015, 32(5).

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      Abstract:C16 Guerbet alcohol (2-hexyl-1-decanol) was synthesized from n-octanol by using supported CuO-NiO catalyst with KOH. The effects of catalyst support, CuO-NiO loading (%) and CuO/NiO molar ratio on the synthesis were investigated so that the best CuO-NiO catalyst was chosen (CaCO3 supported, CuO-NiO loading 30 w% and CuO/NiO molar ratio is 1∶2). Besides, the effects of reaction temperature, reaction time and catalyst dosage (mass percentage of catalyst and n-octanol) on the reaction were studied. The results indicate that C16 Guerbet alcohol is able to be produced in the presence of CuO-NiO catalyst and KOH. When C16 Guerbet alcohol was synthesized under reaction temperature 240 ℃for 1 h with 0.1 % best CuO-NiO catalyst and 3.0 % KOH added, the yield and the selectivity reached 83.5 % and 87.3 %, respectively.

    • Recyclable Magnetic Nano-Triphenylphosphine Ligand: Preparation and its catalytic Property in Hydroformylation Reaction

      2015, 32(5).

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      Abstract:A recyclable magnetic triphenylphosphine ligand was prepared via a surface exchange reaction to load triphenylphosphine onto the surface of iron oxide nanoparticle with dopamine as a linker. The structure of magnetic nano-triphenylphosphine was characterized by IR, elemental analysis and TGA methods. The loading amount of triphenylphosphine on iron oxide nanoparticles could be elevated by increasing the ratio of dopamine-triphenylphosphine over nanoparticle and sonication time. Under the optimized condition, the triphenylphosphine content in the magnetic nano-triphenylphosphine ligand was 0.21 mol/mg. The magnetic nano-triphenylphsophine ligand could catalyze the hydroformylation reaction of styrene with Rh(OAc)2 as a Rh source and the in situ formed magnetic nano-triphenylphosphine-Rh catalyst could be recycled for 4 times under the optimum reaction condition with only 4.8% of triphenylphosphine dropped off from the nanoparticle surface. The optimum reaction condition of styrene hydroformylation was: 1.25 mL styrene, 30 mg nano-triphenylphosphine (0.0063 mmol TPP), 1.8 mg Rh(OAc)2, 12 mL THF, 3 MPa syngas (VCO:VH2 = 1:1), 90 °C, reaction time 9 h.

    • Modification of Cu/ZrO2 catalysts for catalytic hydrogenolysis of glycerol to 1,2-propanediol

      2015, 32(5).

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      Abstract:A series of ZrO2 supported copper catalysts were prepared by impregnation of incipient wetness method and tested in gas phase hydrogenolysis of glycerol to 1,2-propanediol. The pore structure, morphology, crystalline phase and reducibility of the catalysts were characterized by BET, TEM, XRD and H2-TPR, respectively. The effect of support was screened in preliminary tests, where SiO2 was found to be the best in activity and selectivity, but failed in stability; ZrO2was the next in activity, but inferior in selectivity. For purpose of modification, the elements of rare earths like La, Ce, Y were added in ZrO2 by coprecipitation method. The performance of catalysts was obviously improved after doping of La, Ce and Y in ZrO2 support, among which, yttria stabilized ZrO2 (YSZ) was the best. Later, Ce was introduced as a promoter by successive impregnation of Cu and Ce precursors. The best catalyst was found to be 18wt.%Cu-4wt.%CeO2/YSZ, with the yield of 1,2-propanediol over 93%. Instrumental characterization revealed that this catalyst contained an open pore structure and BET surface area 107m2/g, while its CuO crystal was also the smallest in size and easiest to reduce. Time-on-stream test was carried out with the thoroughly optimized catalyst, a 1,2-propanediol yield over 94% was maintained over 1600hr, foreseeing a prospect of commercialization.

    • Dawson structure P-Mo-V heteropolyacid salt catalyst in synthesis of diphenylmethane

      2015, 32(5).

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      Abstract:The heteropolyacid salt Fe2H2P2Mo16V2O62•41H2O catalyst was prepared, and characterized by inductive coupling plasma emission spectrum, Fourier transform infrared spectroscopy, X-ray powder diffraction, and thermal analysis. In this work, the catalytic activity was studied for alkylation of benzene with benzyl chloride to diphenylmethane. The influences of different parameters such as the amount of reactants, the reaction temperature, and the reaction time on alkylation of benzene were also investigated. Experimental results show that Fe2H2P2Mo16V2O62 was found to be a suitable catalyst for the alkylation of benzene with benzyl chloride to diphenylmethane. A maximum of conversion of benzyl chloride was obtained to be 99.5% with selectivity to 98.7% for diphenylmethane under the optimized reaction conditions over Fe2H2P2Mo16V2O62•41H2O.

    • >Perfumes and essences
    • The Comparison of Volatile Flavor Constituents between Traditional Cooking and Flexible Packaging Wuxi Sauce Sparerib

      2015, 32(5).

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      Abstract:The volatile flavor constituents of traditional cooking Wuxi sauce sparerib were extracted by solid phase microextraction (SPME) and simultaneous distillation extraction (SDE), and identified by the gas chromatography-mass spectrometry (GC-MS). Compared with the volatile flavor components of flexible packing Wuxi sparerib, the former 71 compounds were identified and the latter 76 species were identified, and both of the detected have 31 species. The differences in the aldehydes and the sulfur-containing compounds, nitrogen-containing compounds and heterocyclic compounds are more significant, which are the main reasons for the different flavor compounds in two sauce spareribs. In addition, the different fennel and other spices usage may be another cause of traditional cooking and flexible packaging Wuxi sauce sparerib flavor differences.

    • >Drug and cosmetic materials
    • Synthesis and Biological Activity of Schiff Base Sulfur Ether Derivatives Containing 1,2,4-Triazole Unit

      2015, 32(5).

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      Abstract:Starting from 2,4-dichlorobenzoic acid, 4-amino-5-(2,4-dichlorophenyl)-2H-1,2,4-tria- -zole-3(4H)-thione 4 was afforded in four steps including esterification, hydrazidation, salt formation, cyclization. 5-(2,4-dichlorophenyl)-4-( substituted methyleneamino)-2H-1,2,4-triazole- 3(4H)-thione 5 was then synthesized by the condensation reaction of the intermediate 4 with substituted formaldehyde. Eight schiff base sulfur ether derivatives containing 1,2,4-triazole unit in yield of 69%~78% were synthesized by reaction of 5-(2,4-dichlorophenyl)-4-( substituted methyleneamino)-2H-1,2,4-triazole-3(4H)-thione with halogenated hydrocarbon using K2CO3 as catalyst in acetonitrile at 75℃ for 2 h. The structures were confirmed by 1H NMR, 13C NMR, 19 F NMR, IR and elemental analyses. The preliminary bioassay showed that the antifungal activity of some compounds to P.cubensis at the concentration of 100 mg/L was 100%。

    • >Food and feedstuff chemicals
    • Synthesis of Labeled of Tulobuterol - D9

      2015, 32(5).

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      Abstract:This paper presents an efficient synthesis of tulobuterol-D9 with self-made tert-butylamine-D9 as the labeled precursor. Tulobuterol-D9 was synthesized from O-chloroacetophenone as the starting material by bromination with CuBr2, amination with tert-butylamine-D9, reduction with NaBH4. Uniform design method was used to study the effects of the process conditions and experiment data was analyzed by quadratic polynomial regression. The optimized reaction parameters were: reaction temperature is 59 ℃, reaction time is 5 h, dosage of solvent is 25 mL, the molar ratio for bromoacetophenone and t-butylamine-D9 is 1:2. As-synthesized product was confirmed by MS, NMR and HPLC to be target compound. Its chemical purities is higher than 98.0 % and isotopic enrichment is higher than 97.5 %(atom D). The above compound could be used as internal standard in the field of food safety.

    • >Leather chemicals
    • Synthesis and Properties of Waterborne Polyurethane Modified with Epoxy Resin and Castor Oil for Leather Finishing Agent

      2015, 32(5).

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      Abstract:A series of stable waterborne polyurethane for leather finishing modified with epoxy resin and castor oil (ECOWPU) were prepared by the prepolymer process using polypropylene glycol (PPG) and isophorone diisocyanate (IPDI), with castor oil (CO) and epoxy resin(E-44) as the coupling agent. The structure of the polymer and the properties of the resulting films were analyzed by FTIR, TEM, DSC and TGA. FTIR showed that castor oil and epoxy resin were chemically incorporated into the copolymer. Both hydroxyl groups and epoxy groups of epoxy resin participated in the reaction. TEM showed that the particle morphology was spherical, and the particle size was relatively uniform. DSC indicated that the degree of micro-phase separation in the modified films increased. TGA revealed that the thermal properties were better when castor oil and epoxy resin were incorporated. With increase of the content of castor oil and E-44, the tensile strength increased asymptotically, and the elongation at break and the water absorption decreased.

    • >Water treatment technology and environmental protection
    • Photocatalytic Degradation of Organic Dye with H2P6W18O62/TiO2-SiO2

      2015, 32(5):0-0.

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      Abstract:H6P2W18O62/TiO2-SiO2 was prepared by using impregnation method and characterized by FI-IR, XRD and SEM. Through the study of methyl orange with H6P2W18O62/TiO2-SiO2, the optimal conditions found are as follows: H6P2W18O62 loading dosage is 30%, calcination temperature was 200 ℃, calcination time is 3 h. Its activity for photocatalytic degradation of methyl orange in dye waste water was investigated. The influence of initial concentration of methyl orange, catalyst dosage and pH value of solution on photocatalytic degradation efficiency was studied. The reuse of the catalyst was discussed. The results indicate that H6P2W18/TiO2-SiO2 photocatalysts exhibit superior photocatalytic performance, when catalyst dosage is 1.39 g /L and initial concentration of methyl orange is 5 mg /L in the pH=3.5 and the reaction time is 2.5 h under the optimum conditions, the degradation rate of photocatalytic methyl orange is 99.2% and produced a synergistic effect. The photodegradation of methylene blue, rhodamine B and methyl red were also show superior photocatalytic performance, and the degradation rate of dyes can reach 84.0%~100.0%. Photocatalyst also exhibited good reusability and the degradation rate for methyl orange still kept at 94.4% after 5 runs.

    • >Dyeing and finishing auxiliaries
    • Study on Properties and Preparation of Phosphorus-containing Flame Retardant Waterborne Polyurethane Emulsion

      2015, 32(5).

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      Abstract::DOPOMA was synthesized by 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide(DOPO) and  maleic anhydride(MAH), then it with dicarboxylic acids and diols by polycondensation reaction to get the side chain phosphorus hydroxyl-terminated saturated polyester, then it with TDI, DMBA and DEG as chain extenders,TEA as neutralizer to synthesis phosphorus flame retardant waterborne polyurethane. Chemical composition, thermal stability, charring performance, morphology and mechanical properties of phosphorus-containing polymer were investigated by Infrared analysis(FT-IR), Thermogravimetric analysis(TGA), Limiting oxygen index (LOI), Scanning electron microscope (SEM), universal tensiletest machine.

    • >Acrylic series chemicals
    • Synthesis of polyethylene glycol (200) dimethacrylate with light colour

      2015, 32(5).

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      Abstract:Polyethylene glycol (200) dimethacrylate was synthesized by transesterification of polyethylene glycol (PEG-200) and methyl methacrylate. The effects of solvent, catalyst, inhibitor and decolorizer on transesterification were investigated. The results show that the solvent of cyclohexane reduce the reaction temperature and remove the by-product of methanol from the solution easily. The yield can reach 80.2 %, and the colour is 50 APHA, when m(cyclohexane) : m(reaction material) = 2 : 5, m(K2CO3) : m(PEG-200 and methyl methacrylate) = 8.6 : 100, m(MEHQ) : m(PEG-200 and methyl methacrylate) = 1.1 : 100, and m(decolorant A) : m(PEG-200 and methyl methacrylate) = 2.1 : 100.

    • >Fine chemical intermediates
    • Kinetic Resolution of 3,3,5-Trimethylcyclohexaone over Pd/Al2O3 Catalyst Modified by Monolayer (L)-Proline

      2015, 32(5).

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      Abstract:The Product of isophorone(IP) asymmetric hydrogenation, i.e., chiral (R- or S-) 3,3,5-trimethylcyclohexaone (TMCH), is foremost significance fine chemicals intermediates. In the paper, that the asymmetric hydrogenation of isophorone and the catalytic hydrogenation kinetic resolution of TMCH catalyzed by Pd/Al2O3 catalyst in the presence of (L)-proline was investigated. It was shown that the condensation product formed from the pretreatment of the reaction mixture of isophorone with (L)-proline indeed inhibited the asymmetric hydrogenation of isophorone. The spontaneous monolayer dispersion of (L)-proline appeared very easily on the surface of Pd/Al2O3 catalysts, and this phenomenon could effectively increase TMCH enantiomeric excess (ee) from the hydrogenation of TMCH. The ee % of TMCH hydrogenation product was as high as 100 % from the Pd/Al2O3 catalyst modified by the monolayer dispersion of (L)-proline at 40 ℃, and under hydrogen pressure 1 MPa for 10 hrs.

    • Preparation and Structurally Identification of Dehydroabietyl Imidazoline

      2015, 32(5).

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      Abstract:Based on investigation of the thermogravimetric curve TG/DTG of dehydroabietic acid diethylenetriamine salt (II), a method for preparation of dehydroabietyl imidazoline (IV) has been developed. A solution of dehydroabietic acid (I) in xylene used as water-carrying agent was dropwise added to the hot diethylenetriamine (DETA) to give the product via a high temperature liquid-liquid-short-contact dehydration condensation reaction. The product has a poor solubility in DETA, which is used as the reactant and can regulate reaction temperature; the water produced by dehydration condensation was easily taken out of the reaction system by xylene, which was fast heated and evaporated. The product was easily separated from reaction mixtures via cool crystallization, and structurally identified by means of EA, IR, UV, 1H-NMR and 13C-NMR. Molar ratio of DETA to compound I could change the reaction temperature, which has obvious effect on the yield and color of the product. Under the reaction conditions ( amount of compound I, 30 m mol; molar ratio of DATE to compound I , 15.7; reaction temperature, 210 ℃; reaction time, 4 h),the yield is 86.0 %.

    • Synthesis of 5-(4'-methyl-[1,1'-biphenyl]-2-yl)-1H-tetrazole

      2015, 32(5).

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      Abstract:5-(4'-methyl-[1,1'-biphenyl]-2-yl)-1H-tetrazole was synthesized from 4'-methyl-[1,1'-biphenyl]-2-carbonitrile as the starting material in a total yield of 81%. 4'-Methyl-[1,1'-biphenyl]-2-carboximidamide(3) was firstly obtained by the addition of 4'-methyl-[1,1'-biphenyl]-2-carbonitrile with sodium amide in toluene. The consequent substitution reaction of 3 with hydrazine hydrate resulted in the formation of 4'-methyl-[1,1'-biphenyl]-2-carboximidhydrazide(4), and the final acidic cyclization of 4 with sodium nitrite gave the title compound 5-(4'-methyl-[1,1'-biphenyl]-2-yl)-1H-tetrazole(1), whose structure was characterized by 1H NMR and MS.