• Volume 27,Issue 11,2010 Table of Contents
    Select All
    Display Type: |
    • >Functional materials
    • The synthesis of MnO2 nanorods by cheap template method

      2010, 27(11).

      Abstract (319) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:In this paper, α-MnO2 nanorods were successfully synthesized by chemical solution route with the reproducible,low-cost, porous sawdust as template.The obtained samples were characterized by TEM, FT-IR and XRD tests. The results of the tests showed that the samples were α-MnO2 nanorods with diameters of about 10nm and with lengths up to 150 nm. The super electrochemical characteristics of the samples were characterized by cyclic voltammetry (CV) and constant current charge-discharge tests (CH/DCH). The results demonstrated that α-MnO2 nanorods had excellent electrochemical performance in 1.0 mol?L-1 (NH4)2SO4 electrolyte within the potential range of 0~1.0 V (vs.SCE). The initial specific capacitance of single MnO2 electrode reached 176 F譯-1 and 138F譯-1 at the current of 5 mA and 10 mA respectively.

    • Study on the flame retardancy of polyphenylmethoxy Silicone modified epoxy resins

      2010, 27(11).

      Abstract (336) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Silicone modified epoxy resins were prepared via polycondensation of polyphenylmethoxy(PPMS) and epoxy resin (E-20). The flame retardant properties of cured silicone modified epoxy resins were inverstigated by limiting oxygen index (LOI), UL-94 testing and thermogravimetric analysis (TGA).When the mass ratio of E-20 to PPMS was 7:3, the cured modified epoxy resin exhibits the optimal effect. The LOI value was 21.5%, higher than those of unmodified epoxy resins systems by 4%.The burning rate was reduced from 36.23mm/min to 26.60mm/min. The TGA date indicated that the thermal oxidative degradation process of the cured modified epoxy resin is composed of two steps.The 5% weight loss temperature of degradation was 134.7℃, higher than the unmodified epoxy resins by 28.3℃. The residue weight for the cured modified epoxy resin at the temperature of 750℃ was 25.79%,compared to the original date of 0.21% at 750℃ .The chemical structure of char for the resin at the end of LOI test was analyzed by Fourier transform infrared. Based on above results, the flame retardant mechanism was discussed.

    • Fabrication of SiCf/SiO2 composites and the Influence of Interfaces on the mechanical properties

      2010, 27(11).

      Abstract (642) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:2.5-dimension continuous silicon carbide fiber reinforced silicon dioxide composites (SiCf/SiO2) was fabricated by vaccum infiltration. The effects of different interfaces on SiC fabric preform on the mechanical properties of the composites were studied. The bending strength of the composites, in which the fabric without interface,was 52.2MPa, while coating the fabric with pyrolytic carbon (PyC) and PyC/SiC multi-layer interfaces enhanced the bending strength to 67.4 and 180.3MPa. However, the interfaces also declined the toughness of SiCf/SiO2 composites. The surface morphology of fractured composites was analyzed by Scanning electron microscope. The results show that the interfaces not only increase the bending strength but also enhance the bonding between the matrix and fibers which improves the load transfer from the matrix to the fibers. The PyC/SiC interfaces protect the SiC fibers against being damaged by the water released during the processing of sintering and promote the mechanical properties of SiCf/SiO2 composite.

    • Preparation, Characteristics and Antibacterial Activity of Nano-Ag loaded on Bayberry Tannin-grafted Collagen Fiber

      2010, 27(11).

      Abstract (403) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A novel antibacterial agent (CF-BTx-nAg) of nanometer silver (nAg) was synthesized by using bayberry tannin (BT) grafted collagen fiber (CF) as supporting. Bayberry tannin (BT), a typical natural polyphenol, was grafted onto the CF surface to improve the loading capacity and to control the size as well as the dispersion of Ag nanoparticles. The main physical and chemical properties of this antibacterial agent were characterized by means of Scanning Electron Microscopy (SEM), Fourier Transform-Infrared Spectroscopy (FTIR), X-ray Photoelectron Spectroscopy (XPS) and X-ray Diffraction (XRD). It was found that this antibacterial agent is in highly ordered fibrous state. The average diameter of Ag nanoparticles is 3.25 nm and the nanoparticles are homogeneously dispersed. Antibacterial experiments demonstrated that CF-BTx-nAg exhibited high antibacterial activity. When cell suspensions of Escherichia coil solutions with concentration of ~105 cfu/mL was cultivated with CF-BT0.2-nAg at 310 K under shaking (150 r/min, conc. of Ag = 8 μg/mL), the number of living cells went down to zero within 4 h, while it was 8 h and 12 h for that of CF-BT0.05-nAg and CF-BT1.0-nAg, respectively. The minimal inhibitory concentration (MIC) of CF-BT0.2-nAg against E. coli was 4 μg Ag/mL. In addition, CF-BT0.2-nAg can be re-applicated effectively at least five times. These facts suggested that CF-BT-nAg could be used as a new and effective antibacterial agent.

    • >Surfactants
    • Synthesis and Characterization of Alkyl Polyglucosides Quaternary Ammonium Salt

      2010, 27(11).

      Abstract (557) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:N-(3-chlorine-2-hydroxypropyl)-N,N-dimethyl-N-dodecyl-ammonium chloride (CHPDDAC) was synthesized with N,N-dimethyl dodecyl amine hydrochlorate and epichlorohydrin. Then, Alkyl polyglucosides(APG) was quaternizing modified into Alkyl polyglucosides quaternary Ammonium Salt(APGQAS) by CHPDDAC. The effects on the reaction process were investigated by the orthogonal experiment, The optimum conditions of the APGQAS were obtained as follows: isopropyl alcohol as solvent; n(APG):n(CHPDDAC) = 1.1:1; reaction temperature 80℃; reaction time 7h. The structure of APGQAS was characterized by FTIR spectrum, elementary analysis and 1HNMR. The surface activities of the product were measured, the critical micelle concentration(CMC) is 3.16×10-4mol/L, surface tension is 21.51mN/m, Krafft point is -3.57℃.

    • Synthesis and properties of acetal cationic surfactant containing Benzimidazole

      2010, 27(11).

      Abstract (508) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:[(2 – alkyl-1, 3 - dioxane -4) methyl] - 1 – benzimidazole was prepared through condensation reaction using aldehyde, epoxy bromopropane and benzimidazole as raw materials. The resulting reacted with dimethyl sulfate to afford two acetal cationic surfactants containing benzimidazole of 1 - [(2 - hexyl 1, 3 - dioxane -4) methyl] - 1 - methyl - methyl sulfate benzimidazole (3a) and 1 - [(2 - nonyl 1, 3 - dioxane -4) methyl] - 1 - methyl - methyl sulfate benzimidazole (3b). The optimal synthetic condition of intermediate [(2 – nonyl- 1, 3 - dioxane -4) methyl] - 1 - benzimidazole was: n (capric acetal): n (benzimidazole): n (NaOH) = 1:1.1:4, refluxing for 24h. The yield of intermediate was 52.0%. The surface properties of 3a and 3b were respective measured. The critical micelle concentration were 1.4 × 10-3 mol / L and 1.2 × 10-3 mol / L in 20℃; Krafft points were lower than 20 ℃; Foam stability was 70.2% and 77.4%; emulsification was the 31min and 33min. The structure of intermediate and target compounds were characterized by IR, 1HNMR spectra.

    • >Modernization technology of traditional Chinese medicines
    • Analysis of Volatile Oils Chemical Composition in Different Parts of Humulus scandens (Lour.)Merr. by MAE-HS-SPME

      2010, 27(11).

      Abstract (450) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The volatile compounds were extracted in the different parts of Humulus scandens (Lour.)Merr. by microwave-assisted headspace solid-phase micro-extraction(MAE-HS-SPME). Their constituents were analyzed and identified by gas chromatography-mass spectrometry combined with Kovats retention index, and were quantified by calculating the relative contents basing on the peak areas normalization method. The results showed that 86 volatile constituents in the stem, 90 in the leaf and 103 in the flower of Humulus scandens (Lour.)Merr. were separated and identified. Accounting for 96.690 %、96.443% and 94.097% of the total peak areas, respectively. Which is the main component in stem carvacrol (5.702%), thymol(9.407%),β-caryophyllene(6.884 %) ,α- bergamotene (5.511%),trans-β-farnesene(5.965%),1,3-dimethylbicyclo[3.3.0]oct-3-en-2-one(14.010%) and β-bisabolene (5.798%). And in the leaves β-caryophyllene (12.704%),α-bergamotene (8.588%),trans-β-farnesene (6.662%) and 1,3-dimethylbicyclo[3.3.0]oct-3-en-2-one (7.487%). And in the flowers β- pinene (4.719%), β-caryophyllene (8.201%),trans-β-farnesene(11.906%) and α- humulene(5.515%). It was also observed that there were significant differences in the relative contents of three parts.

    • >Catalysis,separation and purification technology
    • Study on catalytical performance of supported NiB amorphous alloy on hydrogenation of α-pinene

      2010, 27(11).

      Abstract (674) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The supported NiB amorphous alloy catalysts were prepared by the chemical reduction method. Crystalline structures, thermal stability、adsorption property of α-pinene、surface area and acid properties of the catalysts were characterized by XRD,DSC, in-suit FTIR, BET and TPD. The α-pinene hydrogenation reaction was chosen to investigate the catalytic properties and selectivity of the catalysts.The results indicated that α-pinene formed chemical adsorption under synergistic action of NiB amorphous alloy catalysts and supports acid site, acid strength affected catalyst’s selectivity,the percent conversion of pinene is 89.6% by using the supported NiB/ZrO2-Al2O3 amorphous alloy catalysts,the catalyst’s selectivity is 91.2%.After 70h reaction, the percent conversion of pinene reduced by 10% while the catalyst’s selectivity remain virtually unchanged.

    • Furfural Liquid-phase Hydrogenation over CuNi-based Catalysts Derived from Hydrotalcite-like Precursors

      2010, 27(11).

      Abstract (780) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The Cu, Ni-containing hydrotalcite-like precursors were synthesized by co-precipitation, and calcined at 500 oC to obtain the Cu-Ni-based catalysts for furfural (FFR) liquid-phase hydrogenation in the present work. And at the same time, their catalytic properties were also compared with the corresponding Cu-based or Ni-based catalysts, and the effects of reduction activation temperature, hydrogenation temperature, H2 pressure, reaction time and catalyst amount on furfural catalytic hydrogenation were further investigated in details. The used catalysts were also characterized by XRD and H2-TPR techniques. The results showed that Cu and Ni species in catalysts possessed synergistic effect on the furfural hydrogenation. Both furfural conversion and furfuryl alchol selectivity over Cu11.2Ni4.7-MgAlO catalyst could reach up to above 90%, and its catalytic activity had no obvious decrease after being reused 6 times.

    • Research on Extraction of Total Isoflavones from Fructus Sophorae by Microwave-assisted Treatment

      2010, 27(11).

      Abstract (367) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract: In order to gain the optimization extraction condition of isoflavones from Fructus Sophorae by microwave-assisted techniques , we have inspected single factor influence and then optimized them by orthogonal experiment. The results of orthogonal experiment indicated that the yield of Fructus Sophorae isoflavones in the extracts were 52.43% and the purity w(Fructus Sophorae isoflavones)of the products was 36.78% when the liquid-solid ratio of 12.5mL•g-1 at 500 W microwave power at 60 ℃ degree for 7 min.

    • Study on Microwave-surfactant Extraction of Flavone from Trollius Chinensis Bunge

      2010, 27(11).

      Abstract (439) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Microwave-surfactant Extraction of Flavone from Trollius Chinensis Bunge was studied, choose SDS as significant surfactant, and extraction process was optimized by orthogonal experiment. The results showed that the optimum conditions for extracting was: SDS(?=0.75㎎/ml) as extraction agent, solvent amount of 40 ml/g Trollius Chinensis Bunge, microwave power of 600W, temperature of 70℃,extraction for 5 min. Under this condition, extraction rate can be up to 5.35%. Compared with traditional solvent, extraction time was decreased greatly, and extraction rate was increased about 30%.

    • >Perfumes and essences
    • Comparing the Aroma Differences Between Rose Essential Oil Obtained By Different Methods

      2010, 27(11).

      Abstract (489) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:On consideration of comparing the quality of rose essential oil extracted by the methods of steam distillation, solvent extraction, and supercritical CO2 extraction, the essential oil composition were analyzed by GC-MS. The results show that there are 56 components in supercritical CO2 extraction oil, with higher alcohols and esters as the main ingredient, and its esters content was the highest among the three kinds of oil, up to 13%, Besides this, its characteristic fragrance ingredients were as high as 4.568%. Its fragrance was sweet and full, and has a heavy elegant bottom fragrance, of which fatty odor was very light, while faint scent was prominent; The essential oil obtained by steam distillation extraction method has 60 components, with higher alcohol as the main ingredient, up to 78%, and its main aroma components was the highest, which was 71.037%, but its phenylethanol aroma content was only 0.711%, which made it give sweet smell, but slightly thin, with the lack of the honey-like aroma; The essential oil obtained by solvent extraction method has 48 components, with higher alcohols and esters as the main ingredient. Its flavanone classes was relatively high, reaching 4.257%, therefore, its fatty odor was heavy, while fragrance flavor was not outstanding, with poor natural sense.

    • Extraction and Analysis of Volatile Aroma Components in the power of Ziziphus jujuba Mill

      2010, 27(11).

      Abstract (548) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The method of simultaneous distillation-extraction (SDE) was used to extract the volatile aroma components in the power of Ziziphus jujuba Mill. The chosen extracting time was separately 3h, 6h and 9h. One hundred and sixty-nine volatile flavor constituents which included 33 carboxylic acids, 24 esters, 21 aldehydes, 9 ketones, 22 alcohols, 16 heterocyclics, 29 hydrocarbons and 2 phenols were identified from the extractions by GC-MS. The main volatile aroma components identified in the relatively higher peak area percentage(>1%) were dodecanoic acid, n-hexadecanoic acid, tetradecanoic acid, decanoic acid, Z-11-hexadecenoic acid, myristoleic acid, octanoic acid, 2-octenoic acid, nonanoic acid, heptanoic acid, acetic acid, hexanoic acid, furfural, 6,10,14-trimethyl-2-pentadecanone, cis-22-tetradecen-1-ol. By Comparing and evaluating the odor characteristic of the identified compounds, the key odor constituents to the aroma of the power of Ziziphus jujuba Mill are organic acid(acetic acid, hexanoic acid, heptanoic acid, octanoic acid, nonanoic acid), ketone(1-octen-3-one, 1-hydroxy-2-butanone, beta-damascenone), ester(butyl butyrate and hexyl hexanoate), aldehyde(hexanal, nonanal, (E)-2-octenal), phenol(eugenol and 2-methoxy-4-vinylphenol), alcohol(hexanol, benzyl alcohol, alpha.-terpineol) and heterocyclic compounds(furfural, 5-methylfural, 2-acetyl furan).

    • Comparative Research of Different Methods for Quantitative Analysis of Flavor Components in Wine

      2010, 27(11).

      Abstract (533) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The advantages and disadvantages of three kinds of methods such as vacuum distillation-GC, activated carbon adsorption-GC, and HS-GC for quantitative analysis of flavor components in wine were compared in this paper. The experimental results have shown that activated carbon adsorption-GC is proper for detecting acetaldehyde and n-butyl alcohol in wine; vacuum distillation-GC, activated carbon adsorption-GC analysis are fit for measuring n-propyl alcohol and isoamyl alcohol. Besides, it is simple and convenient for analyzing acetic ether, ethyl lactate and methanol by HS-GC. Furthermore, acetic acid and glycerine are suitable for vacuum distillation-GC and activated carbon adsorption-GC analysis, respectively. Due to its moderate boiling point and viscosity, isobutanol can be measured by all three methods. The above conclusions can supply a good reference for later analytical work for flavor components in wine.

    • >Drug and cosmetic materials
    • Synthesis of 4-((4-methylpiperazin-1-yl)methyl)benzoic acid dihydrochloride

      2010, 27(11).

      Abstract (777) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:4-((4-methylpiperazin-1-yl)methyl)benzoic acid dihydrochloride was synthesized from 4-methylbenzoic acid via α-bromination and acidification after aminnation without separation. The effects of the bromine agent and initiator on the bromination and the effects of material ratio, temperature and time on the aminnation were investigated. The optimized conditions were: bromosuccinimide as bromine agent, benzoyl peroxide as the initiator, the yield of 4-(bromomethyl)benzoic acid was close to 88.7%; the ratio of 4-(bromomethyl)benzoic acid to 1-methylpiperazine 1:1.2, sodium bicarbonate as the acid binding agent, the reaction temperature ranges from 20~25℃, the reaction time 8h., the yield of product under this optimum reaction conditions was up to 81.5%. The structure of the product was confirmed by melting point, IR and 1HNMR.

    • >Electro-organic chemistry and industry
    • Study on the formula of the bismuth electroplating solution

      2010, 27(11).

      Abstract (639) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The alkaline electroplating bath formulation of bismuth was developed. The optimal composition formula was obtained by an orthogonal method as follows: bismuth nitrate 60g/L,disodium ethylene diamine tetraacetate(EDTA) 90g/L, 5-sulfosalicylic acid 120g/L, potassium sodium tartrate 60g/L, potassium chloride 60g/L. The influence of bismuth content on the rate of bismuth film and complexing agents on the impact of cathode polarization was studied. The surface roughness, microstructure and adhesion strength of bismuth film was detected. It was the result that the bismuth film has the features of fine and uniform grain, good smoothness, good adhesion and bright color.

    • >Water treatment technology and environmental protection
    • Study on synthesizing PDA with cationicity of 5%

      2010, 27(11).

      Abstract (559) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Using dimethyldiallylammonium chloride and acrylamide as the materials and ammonium persulfate - sodium bisulfate as the initiator, the preparation technologies of copolymer PDA with cationicity of 5% via one-stage addition of the monomers and stepwise increasing temperature were researched by using the intrinsic viscosity as quantitative criterion. The effects of the monomer mass percentage, reaction temperature, Na4EDTA dosage, initiator dosage and maturation temperature on the intrinsic viscosity of product PDA were studied. The results show that intrinsic viscosity of PDA with cationicity of 5% could be up to 19.4dL/g, when the monomer mass percentage was 16%, the reaction temperature was 40℃, the ratio of Na4EDTA mass to monomer mass was 2.0?0-4, the ratio of initiator mass to monomer mass was 7.4?0-4 and the maturation temperature was 60℃. The structure of PDA was characterized by FTIR and NMR.

    • >Dyeing and finishing auxiliaries
    • synthetic and application of flame-retardant phosphoester polysiloxane

      2010, 27(11).

      Abstract (536) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Flame retardant finishing of textiles is one of the hottest topics in recent years. In this study, flame-retardant phosphoester polysiloxane (PPSO) was synthesized by N-β-aminoethyl-γ-aminopropyl polydimethylsiloxane (ASO-1), epoxy chloropropane and tributyl phosphate. The chemical structure of PPSO and the intermediates were characterized by infrared spectrum (IR) and proton nuclear magnetic resonance (1H-NMR). Then PPSO was emulsified to obtain transparent emulsion. It was found that the average diameter and the Zeta potential of the emulsion is 62.5nm and +53.71mV respectively by the Malven nanometer particle-size and the Zeta potential analyzer. The emulsion was applied to cotton fabric and the fishing effects of flame retardant agents usage was investigated. Research shows that finished cotton fabric had flammability. The Optimum dosage of the flame retardant was 200g•L-1. By using Thermogravimetry Analysis (TGA), the pyrolysis process of cotton fabrics was studied to explain the flame retardant mechanism of cotton fabrics. The results showed that flame retardant caused fibers to dehydrate and carbonize, increasing the char yield.

    • >Oil field chemicals and petroleum additives
    • Microwave -Promoted Synthesis of Di-esters of Adipic Acid and Azelaic Acid without Solvent

      2010, 27(11).

      Abstract (419) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Under microwave irradiation the di-esters of lubricating oil are synthesized by the reaction of adipic acid or azelaic acid with 2-ethylhexyl alcohol or dodecanol. The results show that for catalyst amount of 3.0% ~3.5% and microwave power of 300 w~320 w the yields of di-(2-ethylhexyl)adipate and di-(2-ethylhexyl) azelate are respectively 99.4% and 98% for 12 min and 8 min, and the yields of didodecyl adipate and didodecyl azelate are respectively 97%and 95% for 6.5 min and 7.5 min. The experimental parameters of microwave synthesis for four di-esters are investigated. The chromaticity and crystallization point of di-esters are measured and their structures have been characterized by 1H NMR、13C NMR and IR spectra. Compared with conventional synthesis method, the microwave method can achieve excellent yield of 95%-~99.4% within 6.5 min -~12 min. The reaction time has a reduction by a factor of 7.1 to 11.4 and the yields of didodecyl adipate, didodecyl azelate, di-(2-ethylhexyl) adipate and di-(2-ethylhexyl) azelate are 3%, 6%, 11.5% and 29% higher than the conventional yields, respectively. Moreover, the color of products is colorless or white. Microwave synthesis method is a rapid, highly efficient and novel synthetic approach for lubrication oil di-esters.

    • >Special dyes and pigments
    • The Synthesis and Spectral Properties of Tetra-(3,4-dimethoxyphenyl)dithiolene Nickel Complex

      2010, 27(11).

      Abstract (1298) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:In this paper, the tetra-(3,4- dimethoxyphenyl)dithiolene nickel complex was synthesized by sulfuration with P2S5 and nickel complexation by using bis-(3,4-dimethoxy-phenyl) ethanedione as raw materials. The structrure of the final product dithiolene nickle complexes were characterized by IR and 1H-NMR. The maximum absorption wavelengths of tetra-(3,4-dimethoxyphenyl) dithiolene nickel complex in different solvent and its photo stability and thermal stability were investigated.

    • >Building chemicals
    • Synthesis of Methylnaphthalene Sulfonic Formaldehyde Polycondensate

      2010, 27(11).

      Abstract (474) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Methylnaphthalene sulfonic formaldehyde condensate (MNSF) was synthesized from industrial methylnaphthalene by four steps: firstly sulfonated by H2SO4, then hydrolysised by H2O, nextly condensated by HCHO and neutralized by NaOH. The factors influencing the dispersion ability of MNSF used as superplastiser were investigated. The optimum reaction conditions were described as below: the mole ratio of material is n(methylnaphthalene): n(H2SO4): n(H2O of hydrolysis): n(HCHO):n(H2O of condensation) =1:1.25:1.25~1.5:0.92:4.6; sulfonation temperature was 160~165 ℃; sulfonation time was 3h, hydrolysis temperature was 110~120℃; hydrolysis time was 15~30min; condensation temperature was 110℃; condensation time was 4 h; the acidity value before and after hydrolysis was controlled near 30%. When the dosage of MNSF was 0.5%, the water-reducing ratio reached to 16% and 4% more than that of FDN, the flexural and compression strength of added MNAF cement mortar approached that of FDN.

    • >Fine chemical intermediates
    • Studies On The Synthesis Of Aniline

      2010, 27(11).

      Abstract (977) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:We study the synthesis of 9, 9-bis (4-aminophenyl) fluorene(BPF) and the effects reaction conditions such as different acid catalysts, mass of acid catalyst, mass of aniline, reaction temperature and reaction time on the yield of BPF were discussed. The test results showed that dehydarted by appropriate amout of toluene when n(aniline):n(HCl):n(fluorenone)=10:1.5:1, reaction temperature is 130 ℃, reaction time is 6 h, we can gain the highest rate of BDF to 88.3%.

    • Synthesis of p-(trifluoromethoxy)-N- ethoxyl-benzenaime

      2010, 27(11).

      Abstract (399) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract:P-(trifluoromethoxy)-N-hydroxyethyl-benzenamine (3) was selectively synthesised using p-(trifluoromethoxy)-benzenamine (1) as the raw material . The product was obtained by the route during amidation with chloroethyl chloroformate,then hydrolyzed and rearrangement in NaOH aqueous solution,the structure of products were confirmed by 1H NMR,13C NMR,Ms and IR.Factors on yield of products were studied,it was found that the yield of 3 can reach 93.7% under the optimal reaction condition of n(NaOH):n(amide) with 5:1 at 50℃ for 7h in dioxane . Keywords:p-(trifluoromethoxy)-N- hydroxyethyl-benzenamine;p-(trifluoromethoxy)-benzenamine;chloroethyl chloroformate;synthesis Foundation item:Natural Science Foundation of China(20905057)