Abstract:Seven ferrocenyl schiff base organometallic compounds with third-order nonlinear optical properties which had large π-conjugated systems were designed and synthesized starting from ferrocene and substitutional amine. The process of reactions were discussed and the conditions of the reactions were selected. The results showed that the optimal parameters were as follows: catalyst alkaline Al2O3, solvent xylene, reflux 10 h. The yield was 59.1% .The influence of different substituted amine on the reaction yield was compared. It was concluded that the amine with more intense basicity give the higher yield. All the compounds were characterized by 1H NMR，MS and UV．The synthetic methods were simple and feasible.

Abstract:High-performance NaA zeolite membrane was synthesized on polyetherimide(PEA)-NaA zeolite/α-Al2O3 composite supports by microwave heating method. Influence of microwave heating time on membrane synthesis was mainly investigated. The as-synthesized NaA zeolite membranes were characterized by XRD and SEM. XRD results show that only NaA zeolite emerges on the composite support surface. The SEM results show the composite support surface is fully covered by uniform and compact NaA zeolite membrane. The pervaporation properties of the as-synthesized membrane were evaluated by dehydration of alcohol/water mixture. It was found that the flux decreased with the increment of the alcohol amount in the feed, separation factors were on the contrary. Pervaporation results present that separation factors were as high as 13000 at m(C2H6O) /m (H2O) = 95:5, instead, the fluxes were only 0.05 kg/(m2?h).

Abstract:Sodium single-fatty alcohol phthalate ester was synthesized with phthalic anhydride and different alcohol under catalyst and then neutralized with sodium hydroxide. The influence of catalyst, alcohol, rate of material, esterification temperature and solvent were investigated, and structure, foam capacity and interface were also studied in the paper. The optimum reaction conditions of esterification condition was catalyst for self-made BN-1, xylene as solvent, n(alcohol):n(phthalic anhydride)=1:1.60, esterification temperature 100℃, esterification time 5h. As the alcohol carbon chain increased, the product of a single phthalate ester sodium salt foam capacity gradually decreased, but the ultra-low interfacial tension increased gradually.

Abstract:Adipic acid is synthesized by means of a “one-pot” reactive mode with cyclohexene and hydrogen peroxide(w=30%) using modified catalyst 400PW/SBA(40)（brief note PW/SBA）. The process is the scientific method of clean synthesis becauce of no organic solvents. Three steps were taken in the study to optimize the conditions of the synthesis process of adipic acid. First of all, the basic route of synthesizing adipic acid was determined by pre-experiment program. Then the orthogonal experiments method and the single factor test method was used to optimize the conditions of reaction process. Finally, the better process of synthetic routes and conditions was tested by using the parallel experiment methods . The obtained condition is reaction time 12h, temperature 80℃, the amount of catalyst 1.75g, n(H2O2): n(cyclohexene)=5.47:1, adding the amount of another 1/2H2O2 after reaction time is 3.5h. The results indicate that the yield of adipic acid could reach 74.5% , and purity quotient 99.7% under the optima condition. Moreover, characterized N2 adsorption–desorption isotherms and BJH cumulative pore volume of the PW/SBA were investigated.

Abstract:MgO/La2O2CO3 catalyst prepared by thermal decomposition of the precursors obtained from coprecipitation method was tested in low-temperature OCM (oxidative coupling of methane). The result showed that such catalyst could hold the reaction for at least 24h at Tex=50 oC (external furnace temperature). The addition of Ni2 to the catalyst caused lower Ti (ignition temperature) and Tm(minimum reaction temperature) of OCM reaction, which was due to the enhancing catalytic performance of Ni2 on COx selectivity in OCM. The addition of Zn2 promoted the C2 selectivity, but brought negative impacts on the reaction exothermicity, which led to the lower stability of the catalyst. The thermal effects of the OCM accompanying side reactions to produce COx played great role on the process of the low temperature OCM reaction. The component La2O2CO3 was believed to provide the main active species for the reaction.

Abstract:Abstract: Four cobalt–deuteroporphyrins were synthesized and used as catalysts for cyclohexane oxidation with air in the absence of additives and solvents. The four kinds of cobalt–deuteroporphyrins show good catalytic performance when temperature was 150 ℃, Catalyst: substrate ≈ 1:4.63 × 105 (mol / mol) and pressure was 0.80 Mpa. Substrate which used four kinds of cobalt–deuteroporphyrins as catalysts, its conversion rate within 4 h had reached more than 14% and the target product alcohol and ketone were formed over 82% selectivity. The catalytic activity of cobalt-3,8-dinitro deuteroporphyrin dimethyl ester was superior to another three kinds of deuteroporphyrins. The alcohol and ketone were formed to 82.30% selectivity at a cyclohexane conversion of 19.34% under the optimum conditions, and turnover number reached to 8.86×104.

Abstract:The volatile flavor compounds from Dongbei lentinus edodes were extracted by simultaneous distillation and solvent extraction (SDE) of 2h, 4h and 6h. The extracts were analyzed by GC-MS using the polarity column DB-WAX. Total of one hundred and thirty -seven volatiles were identified, which included ten oxygen-containing heterocyclics, thirty-six sulfur-containing compounds, twenty-one nitrogen-containing heterocyclics, eleven phenols, ten aldehydes, eight ketones, twelve alcohols, three long-chain fatty acids and twenty-six hydrocarbons. Comparing the yield, odor characteristics and flavor compounds identified in GC-MS from the extract using different SDE times, the SDE of 6h was considered optimal. In this condition, the extraction yield was 0.51% and the extract had strong lentinus edodes aroma while the flavor components identified in high amount were 3,5-dimethyl-1,2,4-trithiolane (4.20%), dimethyldisulfide, (3.07%), 1,2,4,6-tetrathiepane(3.33%), methyl(methylthio)methyl disulfide (2.34%), 1,3,5-trithiane (2.22%), 1-(2-thienyl)-ethanone (2.21%) and 1-octen-3-ol (2.03%).

Abstract:Starting from resorcinol and p-methoxylphenylacetic, a facile one-pot synthesis of 7-Hydroxy-4’-methoxyl-isoflavone (Ⅰ) was achieved in 84.0％ yield under ultrasonic irradiation for the first time in the presence of boron trifluoride-diethyl ether, DMF and methanesulfonyl chloride. Then (Ⅰ) reacted with benzoyl chloride, acetyl chloride, 2-phenoxyacetyl chloride, cinnamoyl chloride and 2-hydroxybenzoyl chloride to give five isoflavone derivatives (Ⅱa~e) respectively in 57.1％, 60.6%, 59.4%, 61.1% and 50.4%. Their structures were confirmed by IR, H1 NMR, C13 NMR and MS spectroscopy. Finally the pharmacological assays of anti-osteoporosis indicated that these compounds could promote the proliferation of rat’s osteoblast in vitvo to a certain degree.

Abstract:In order to search a novel PTP1B inhibitor, [2´-bromo-6´-(ethoxymethyl)-3´,4´-dimethoxy-phenyl]-(2,3-dibromo-4,5-dimethoxy-phenyl)-methanone 8 was synthesized in 7 steps with an overall yield of 21.9%, employing bromination, Friedel-Crafts reaction and nucleophilic substitution reaction as key steps. The structure of compound 8 was determined by 1H-NMR, 13C-NMR and infrared absorption spectra. Compound 8 was screened against protein tyrosine phosphatase 1B (PTP1B) with the colorimetric assay. The result indicated that compound 8 displayed good inhibitory activity against PTP1B (Inhibition 73.83% at 20 mg •L-1).

Abstract:The synthesis of a new-type antioxidant of feruloyl-oleylglycerol through lipase-catalyzed irreversible transesterification of vinyl ferulate (VF) and triolein (TO) was studied. Vinyl ferulate made the transesterification reaction irreversible. The structure of VF was identified by NMR and MS and the influential factors of substrate molar ratio, reaction time, reaction temperature, enzyme amount and water activity were systematically studied. Results indicated that in the toluene reaction system the optimal conditions are as follows: n(VF)∶n(TO)=1∶3, reaction time: 62 h, reaction temperature: 55℃, enzyme amount: 20 mg/mL and water activity(aw): 0.07. Under the optimal conditions, the maximum yield as high as 96.73% was obtained.

Abstract:Starch-based carbon was prepared by incomplete carbonation of starch and characterized by powder X-ray diffraction, TGA-DSC, infrared spectroscopy and BET. The adsorptions of Cu2+, Pb2+, Cd2+ and Zn2+ on the starch-based carbon were investigated. The effects of adsorbent dosage, pH value, adsorption temperature and initial metal concentration on the adsorption capacity were investigated in detail. The removal percentages of heavy metal ions increased with adsorbent dosage increase. The optimum pH values were found to be 7.0 for Cu2+, 6.0 for Pb2+, 8.0 for Cd2+ and 8.0 for Zn2+, respectively. Higher temperature was in favor of adsorption. The adsorption behaviors were well fitted to the liner Langmuir isotherms equation.

Abstract:In the presence of N,N'-dihexadecyl-N,N,N',N'-tetramethyl ethyl diamine bromide (21631) and fluorinated fatty alcohol polyoxyethylene ether as emulsifiers and ammonium persulfate as a water soluble free-radical initiator, a novel cationic fluorinated long alkyl polyacrylate FA-co-SLMA-co-DM-co-HPA (FSLDH) emulsion was prepared by copolymerization of perfluoroalkylethyl acrylate (FA) with octadecyl/dodecyl methacrylate (SLMA), dimethylaminoethyl methacrylate (DM) and 2-hydroxypropyl acrylate (HPA) in mass ratio of FA : SLMA : DM : HPA = 80 : 16.5 : 3 : 0.5 in aqueous medium. Chemical structure of FSLDH was characterized by infrared spectrum (IR) and 1H nuclear magnetic resonance (1H NMR), then film morphology as well as the hydrophobic performance property of FSLDH emulsion on cotton fiber substrates were investigated by atomic force microscope(AFM) and X-ray photoelectron spectroscopy (XPS) and other instruments. The experiment results indicate that the FSLDH emulsion could form a macroscopic smooth film on the treated cotton fiber surface. Four elements such as F, O, N, C could been examined on the treated cotton fiber surface. In addition, FSLDH could confer the treated cotton fabric with excellent water- and oil-repellency. When the dosage of FSLDH emulsion reached 5g in 100g H2O, the water- and oil-repellency of the treated cotton fabric respectively reached 90 and 5 degree, and the water static contact angle on the treated fabric surface also reached 144.9º.

Abstract:1-lsopropyl-4-methylbicyclo[2,2,2]oct-5-ene-2,3-dicarboxylic anhydride(TMA) was prepared via isomerization of terpineol-products followed by Diels-Alder reaction with maleic anhydride in the presence of phosphate catalysis. The optimum conditions were found by orthogonal tests to be as follows: reaction temperature 155 ℃, catalyst mass fraction of 1.5%, catalysts mass fraction of 0.08%, n ( by-product of principal component): n (maleic anhydride) = 2.2:1, and reaction time of 2 hours.The yield of TMA amounted to 86.2% .The structure of the TMA was analyzed and characterized by IR, NMR and MS.

Abstract:CoBPcN6 was synthesized respectively using trimellitic anhydride, pyromellitic dianhydride, urea, CoCl2 •6H2O as starting materials and ammonium molybdate as catalyst in BPBF4 , and then hydrolysed to CoBPcC6 under alkaline conditions. The products were characterized by IR and UV-Vis、1HNMR and elemental analysis etc. . The main factors which affect the yield of CoBPcN6 were investigated by Orthogonal test. The results indicate that the optimal conditions are as follows: V (BPBF4) = 60mL, n (PMDA): n (urea) = 50, T = 200 ℃, t = 2h . Compared with conventional liquid phase, it not only avoids environmental pollution caused by the use of conventional organic solvents, but also can be used repeatedly without reducing the activity.

Abstract:The dioscin was extracted from dry yam powder with alcohol in this experiment. After hydrolysis reaction, filtration, neutralization, dehydration, extraction using petroleum ether and recrystallization, high purity diosgenin was obtained. Results of intermittent extraction process show that after three times extraction for 2h-1h-0.5h, the yield of diosgenin can reach 2.45%, using the solvent of 95%(volume content) alcohol, at the liquid-solid ratio 5:1 and temperature 60℃. Continuous homogeneous extraction process was also researched to increase extraction efficiency and facilitate continuous production. The research shows that continuous homogeneous extraction at pressure 60MPa can achieve equal effect to intermittent extraction. Acid consumption and waste water of intermittent extraction and continuous homogeneous extraction decrease dramatically compared to the traditional process, and the yield of diosgenin increases.

Abstract:5,6-Diaminobenzimidazolone-2 is obtained in an overall yield of 62.1% by nitration of benzimidazolone-2 and followed with hydrogenation. Single-factor experiments were conducted to optimize the reaction condition. 5,6-Dinitrobenzimidazolone-2 was synthesized by Nitration of benzimidazolone-2 under 0℃,8h,n(nitric acid)∶n(benzimidazolone-2)=2.2 in 69% yield. 5,6-Diaminobenzimidazolone-2 was made in absolute alcohol in 90% yield by 8h of Raney-Ni catalytic hydrogenation of 5,6-dinitrobenzimidazolone-2 under the condition of 100℃、2.5MPa、m(catalyst)∶m(5,6-dinitrobenzimidazolone-2)=9%.MS、HPLC、IR、1H-NMR、13C-NMR and elemental analysis are properly used for characterization of the structures of the product.

Abstract:1,2-diphenoxyethane with high purity was successfully synthesized by reacting 1,2-dibromoethane with phenol in the aqueous KOH solution. Under the optimized reaction conditions, the molar yield of 1,2-diphenoxyethane exceeding 75% on the basis of 1,2-dibromoethane and GC purity exceeding 99% were achieved, and this attractive result was confirmed by a series of scale-up test with 10kg/batch size. The following optimized con-ditions were obtained: the optimized reaction time is 25h, the concentration of base is w(KOH) = 50%, and the molar ratio of the main reactants is n(KOH): n(phenol) : n(1,2-dibromoethane) =3.0: 3.0: 1.0, the reaction temperature is 60℃. With the above opti-mized conditions, the impurity contained in the final product can be decreased to a limited level.