Abstract:Some different proportions of the sol-gel casting solutions were prepared by adding tetraethyl orthosilicate (TEOS) to the mixed polymerthe of quaternized polyvinyl alcohol (QPVA) and poly dimethyl diallyl ammonium chloride (PDADMAC) aqueous solution for the sol-gel reaction. Then each of the casting solutions in the mold was dried to obtain the hybrid membrane. After that the hybrid membranes were cross-linking in the glutaraldehyde solution with acetone to obtain a dimensionally stable hybridization anion-exchange membrane. The effect of the mass ratio of the quaternized polyvinyl alcohol to poly dimethyl diallyl ammonium chloride casting solution on the stability of the hybrid membrane was investigated. The topography, infrared spectroscopy, morphology, thermal stability, the rate of aqueous/methanol, and the ion exchange capacity of four dimensional stability anion-exchange membranes were mainly analyzed. The results showed that the basic hybrid membrane of QPVA/0.25PDADMAC/0.1TEOS was dimensionally stable in methanol, dense in the microstructure, and excellent heat stability in 65-140℃. Meanwhile, the ion exchange capacity could be reached to 1.09141mmol/g, and the basic hybrid membrane had potential applications in alkaline direct methanol fuel cell with low temperature.

Abstract:We chose octyl-grafted alginate-amide as capsule material to prepare water suspension nanocapsule made of λ-cyhalothrin based on micro-emulsion template. The morphology of nanocapsules was characterized by transmission electron microscopy; the size of nanocapsules was characterized by laser particle size analysis and the effects of different octyl-grafted alginate-amide derivatives, calcium chloride and the amount of surfactant on the sizes of nanocapsules were discussed with the analysis of capsule particle sizes by laser particle size analyzer; moreover, the release performance of the nanocapsules was studied by the release quantity of λ-cyhalothrin determined by gas chromatography. The results indicated: the size of nanocapsules decreased with the increase of surfactant content; the average size of water suspension nanocapsules was 7.76nm when w (λ-cyhalothrin) =2.5%, w (surfactant) =17.5%, w (octyl-grafted alginate-amide derivative) = 1‰ and w (calcium chloride) = 0.5‰; in order to obtain 60% of release rate of chlorine fluorine cyanide chrysanthemum ester with high performance, the micro-emulsion needed 200min and the nanocapsule needed 300min. In all, the nanocapsules restrained the release of core drug.

Abstract:The surface properties, alkaline and stability of dodecyltrimethylammoniu- m hydroxide (DTAH), sodium dodecyl benzene sulfonate (SDBS) and their mixed system were studied. Result showed that when the molar ratio of DTAH and SDBS was 9:1, the mixed system was improved significantly in reducing the surface tension of the capacity and efficiency, and has good stability and strong alkaline. The critical micelle concentration (cmc), surface tension at cmc (γcmc) and pH value of blend system are 3.02×10-5mol•L-1, 28.10mN•m-1 and 12.46 respectively. Interaction parameter in surface (βσ) and micelles (βm) of DTAH/SDBS mixed system achieved -18.36, -22.69, which reflected good synergism.

Abstract:Selective oxidation of cyclohexene was carried out using tin deuterporphyrin dimethyl ester as catalyst with dioxygen. The effect of various reaction parameters, such as reaction time, temperature, pressure and the amount of the catalyst on the conversion of cyclohexene and the selectivity of product on the catalytic performances, was investigated in detail as well as online analysis by GC-MS detection. It was demonstrated that under optimal reaction conditions like 100 ℃, 0.8 Mpa, 7 h, 0.5 mg (7.6?0-4 mmol) catalyst and 10 mL (98 mmol) cyclohexene, the conversion of cyclohexene and the total selectivity of the corresponding product(2-cyclohexen-1-one and 2-cyclohexen-1 -ol) were 84% and 94%, respectively. Furthermore, the reaction mechanism of catalytic oxidation reaction was also preliminarily discussed.

Abstract:Dendrimer chemistry is one of the most fascinating and rapidly expanding areas of modern chemistry. However, solution-phase synthesis of dendrimers is often challenging requiring long reaction time and tedious purification process, which dramatically limits the applications of dendrimers. In this work, polyamidoamine dendrimers were grafted to silica surface through solid phase synthesis methodology, the peripheral amino groups on these dendrimers were modified by 4-hydroxybenzaldehyde, 2,4-dihydroxybenzaldehyde and salicylaldehyde to obtain ligands, and then reacted with SnCl2•2H2O to obtained silica supported dendritic Sn complexes. The ligands and complexes were well characterized by elemental analysis, IR, ICP and XPS. The catalytic performance of the silica supported dendritic Sn complexes was investigated by Baeyer–Villiger oxidation of cyclic and acyclic ketones to their corresponding lactones or esters with 30 % hydrogen peroxide. It was shown that all the complexes exhibit promising catalytic activities for the oxidation. Under the mild condition, all the oxidations give high conversion and selectivity of lactones or esters. The effects of the supporter and ligand on the catalytic activity were also studied, it was discovered that both supporter and the ligand played a vital role in metal loadings and the catalytic activity of the complexes. Moreover, the catalysts could be obtained in a simple and efficient manner and can be recycled and reused.

Abstract:To improve the extraction yield of succinic acid which produced by microbial fermentation, trioctylamine /octanol was used as extraction agent to extract succinate form fermentation broth. The pre-treatment of fermentation broth as well as preparation of succinic acid ammonium using ammonia to re-extraction were investigated. Results showed that the rate of succinic acid extraction from fermentation broth pre-treated by cation exchange resin reached 91.3%, which was higher than that of by sulfuric acid. Aammonia was an excellence re-extraction agent and the extractant (trioctylamine /octano) could be reusable. When extractant was recycled five times, both average rates of extraction and re-extraction were 90.4% and 94.8%, respectively, indicating no obvious changes.

Abstract:A new technology of coupling reaction was studied, which simultaneous synthesis of Poly(ethylene glycol succinate) oligomers and dimethyl carbonate were obtained by coupling reaction of ethylene carbonate and dimethyl succinate over various metal ethyl acetoacetate complexs. Zn(EAA)2 as catalyst has the highest catalysis activity for the coupling reaction. The preferable reaction conditions were follows: reaction temperature 205~215℃, molar ratio of EC to DMSu 4, molar ratio of catalyst to the total mass of EC and DMSu 0.1%, reaction time 1h. under these conditions, the yield of DMC was 52.3%; the intrinsic viscosity [η] of Poly(ethylene glycol succinate) oligomer was 0.1174dl/g.

Abstract:Corncob lignin was extracted with formic acid /acetic acid aqueous solution. The Response Surface Methodology (RSM) analysis was used to study the effects of process parameters on the lignin yield and the optimized condition (formic acid/acetic acid ratio of 4/5(V/V), 91 ℃ and 4 h) was established. The highest yield of lignin was predicted to be 67.91 % by the RSM model and revised to be 70.16 % by the experiments. The purity of obtained lignin, the contents of phenolic hydroxyl and carboxyl group were determined using differential UV-Spectroscopy method ( method) and chemical titration. The complex structures of the obtained lignin were further characterized by FTIR, UV, TG, 1HNMR and compared with that extracted with alkali. The results showed that the lignin is composed of guaiacyl unit (G), syringyl unit (S) and p-hydroxyphenyl unitl (H) and is quite similar with the alkali one in structure. The thermogravimetric analysis showed that the lignin extracted with organic acid queous solution is thermally more stabile than the alkali one and the char residues at 600 ℃ was 42 %. Extraction of lignin from corncob with organic acid aqueous solution was proved to be an efficient method.

Abstract:A new environmental friendly catalyst, H3PW12O40/SiO2 was prepared with the sol-gel method, and characterized by FT-IR and XRD. Cyclohexanone ethylene ketal was synthesized from cyclohexanone and ethylene glycol using H3PW12O40/SiO2 as the catalyst. The influence factors on the yield of cyclohexanone ethylene ketal were also discussed. The optimum conditions were indentified: molar ratio of cyclohexanone and ethylene glycol is 1:1.3, mass fraction of catalyst to reactants is 1.2%, cyclohexane dosage is 3 mL and reaction time is 45 minutes. The yield of cyclohexanone ethylene ketal can reach 89.7% under the optimum conditions.

Abstract:The influence of the storage method of Chimonanthus praecox (L.) Link(CPF)., which were kept under frozen and dryness conditions, respectively, on the quality of essential oils had also been studied. The results showed that the yield and the fragrant components of essential oil from the frozen flower were very similar to the fresh flower. As the frozen time increased, the main fragrant components of CPF kept unchanged, but their contents showed a nonlinear decreasing trend which accelerated significantly after two months of cryopreservation, suggesting that CPF should not be stored for longer than two months under frozen conditions.

Abstract:Using 3-Pyridine carboxylic acid as materials, 3-pyridine carbonyl chloride was obtained via acylation reaction. The acylated α - amino acid reacted with methanol to generate the corresponding amino acid l ester hydrochloride. At room temperature, using triethylamine as deacid reagent, the target products that N- ( 3- formyl pyridine ) -proline methyl ester was obtained at the acylation reaction of 3-pyridine carbonyl chloride with amino acid ester. The structures of all the compounds were confirmed by 1H NMR、13C NMR、IR、HRMS spectra. Then the applications of the ester in cigarette flavoring were studied as well. More than 40 kinds of pyrolysis products were authenticated. Most of the pyrolysis products were aroma components. The smoke panel test showed that the new compound could improve the cigarette taste and flavor, reduce smoking irritation of cigarette.

Abstract:The nitrite scavenging capacity of extracts from Pteridium aquilinum var. latiusculum was evaluated in vitro by spectrophotometric method. On the basis of single factor tests, response surface analysis was designed by Design-Expert Software 8.06. The effects of extraction time, ethanol concentration, ratio of liquid to solid, and temperature on the nitrite elimination were investigated. The results showed that the optimal extraction conditions were as follows: with 71% ethanol as the extraction solvent and a ratio of liquid to solid of 69 ml/g, extraction at 81℃ for 90 min. The predicted of elimination of sodium nitrite was 69.50%, close to the practical elimination of sodium nitrite was 70.21%.

Abstract:Polyvinylidene fluoride (PVDF) hollow fiber membranes were prepared via thermally induced phase separation (TIPS) method by using diphenyl ketone (DPK)-N, N-dimethyl acetamide (DMAc) as diluent and phenolphthalein polyethersulfone (PES-C) as additive. The structure of membrane was observed through SEM and pure water flux, sewage flux, COD and NH4+-N content of MBR effluent were also investigated. A thinner skin layer and porous support layer were formed when 2% PES-C was added into casting solution. Compared with PVDF membrane, the pure water flux of membrane prepared with 2% PES-C addition increased by 60 percent and the sewage flux increased by 37.8 percent, well COD removal ratio of the effluent increased by 3.32 percent and NH4+-N removal ratio increased by 2.2 percent and also the effluent of the membrane came up the discharge standard.

Abstract:Alkaline Ca-bentonite (ACB) was investigated to remove Methylene blue (MB) and Congo red (CR) from aqueous solution as a function of adsorbent dosage, contact time and temperature, initial pH and salt. The adsorption isotherms and adsorption kinetics of the two dyes on ACB were also studied. The main results are as follows: MB and CR removal by ACB increased with the increase of adsorbent dosage. Under experimental conditions, the optimum adsorbent dosage for 50 mg/L MB and 100 mg/L CR were 1.0 g/L and 2.0 g/L, respectively; The elevated adsorption temperature contributed to accelerate the adsorption rate of MB and CR on ACB, but it had little impact on the final decolorizing rate of MB and CR；For 50 mg/L MB and 100 mg/L CR with the optimum adsorbent dosage of ACB, the adsorption equilibrium time were 60 min and 120 min, respectively. The decolorizing rate of MB by ACB remained about 99% when the initial pH increased from 3 to 12, and that of CR by ACB remained about 90% within the optimum pH range 3-7.The addition of NaCl had little effect on MB adsorption but suppressed CR adsorption obviously. MB adsorption on ACB followed both the Langmuir model and the Freundlich model, but CR adsorption on ACB followed the Langmuir model better.The adsorption process of MB and CR can be better described by the pseudo-second-order model than the pseudo-first-order model. The intraparticle diffusion model studies indicated there was pore-filling by diffusing during the adsorption process.

Abstract:Abstract:1-methyl-4-hydroxymethyl-1-silicone miscellaneous-4-phosphorus miscellaneous-2,6,7 -trioxabicyclo[2,2,2]-octane quaternary phosphonium sulfate,a kind of cage-shaped organosilyl quaternary phosphonium as flame retardant antistatic agent was synthesised by methyl trichlorosilane react with tetrakis hydroxymetyl phosphonium sulfuric. We discuss the impact of the reaction temperature、reaction time and resolvent on the yield, and we designed a new production route, which is the molar ratio of methyl trichlorosilane and tetrakis hydroxymetyl phosphonium sulfuric was 2:1, the reaction time was 8h at 120℃,and diethylene glycol dimethyl ether was used as solvent.The synthesized compound has been ascertained by FTIR、1H-NMR.DTA、Limiting oxygen index and surface resistance were used to characterize the performance of the final product. Further research of the product shows the decomposition temperature is 478.5℃, which has excellent flame retardant antistatic performance in the application tests.

Abstract:Through the pad method pure cotton was finished with a novel intumescent flame retardant imidazole spirocyclic phosphoramidate synthesized by ourselves. The influence of the proportion of flame retardant and other assistant agents and the curing temperature on finishing cotton limit oxygen index (LOI) was investigated through orthogonal experiment. The vertical burning and tensile performance were tested for eight flame-retardant cotton samples which LOI over 28% and the better flame retardant finishing process was determined. When the finishing liquor consist of 30% imidazole spirocyclic phosphoramidate and 1.5% catalyst and 2%cross-linking agent and the baking temperature was 170℃, the finishing cotton has 33.96% LOI and B1 flame retardant level with 0 s afterflame time and 0 s afterglow time and 64 mm damaged length and 312.50 N breaking force. The thermal gravimetric analysis showed that the finishing cotton’s initial thermal decomposition temperature brought forward 100 ℃, the maximum thermal decomposition rate was reduced, the residue at 600 ℃ increased to 30% from almost 0%. All above results explain that the cotton finished with imidazole spirocyclic phosphoramidate has good flame retardant effect.

Abstract:Through the design of the functional group, a long-chain quaternary ammonium salts of hydrophobic monomer—C18DMMAAC was synthesized. The structure of C18DMMAAC is charactered by 1H-NMR . Hydrophobically associating copolymer HAPAM-18 was synthesized by copolymerization of C18DMMAAC and acrylic acid (AA), acrylamide (AM) in aqueous solution by free radical copolymerization . HAPAM-18 solution have a higher value of apparent viscosity under the condition of n (AM): n (AA): n (C18DMMAAC ) = 74.94:25:0.06 , AA neutralized to 95% by NaOH, monomer concentration 20wt%, initiator concentration 0.05 wt% of the monomer mass, temperature 45 ℃, and reaction time 12h. The study showed that the critical associating concentration of the copolymer solution is 2000mg / L; the polymer solution is sensitive to temperature, and the viscosity reserved rate is to 70.93% at 80 ℃; the polymer solution is pseudoplastic fluid ,but it performs shear tolerance, and viscosity reserved rate is 115% under shear rate sustaining 1 hour. Since HAPAM-18 contains lots of anionic function groups, the salt resistance of the polymer is poor.

Abstract:A hydrophobically associating polyacrylamide was synthesized using AM,AA,C16DM as monomers.The suitable reaction conditions were :w(initiator)=0.3%(based on the total monomers), x(C16DM)=0.5%,x(AA)= 25%，w(total monomers)=20%,pH7~8,reaction temperature 50℃,reaction time 8h,respectively.The structure was characterized by means of elemental analysis and infrared spectrum.At the same time,the results show that,the surface tension of the solution could be reduced to 42.2mN/m,when the mass concentration was 1g/L.The critical associating concentration appeared when the mass concentration was close to 3g/L.The viscosity declined slowly with temperature rose,and the solution had shear thinning.

Abstract:A hydrophobically associating anionic terpolymer PAnBS was prepared by free-radical micelle copolymerization of acrylamide,sodium 4-vinylbenzenesulfonate(SSS) and n-butyl styrene(nBS).The structure of the synthesized polymer was characterized by means of UV, FT-IR, 1H-NMR.The influence of polymerization reaction conditions on the apparent viscosity of the polymerization product aqueous solution was studied.The optimum reaction conditions were determined as follow:mole percentage of nBS,SSS and initiator were 1.5%,9% and 0.1% relative to total monomers,mass percentage of total monomers and surfactan(SDS)were 25% and 6%;the reaction temperature and reaction time were 50℃ and 10h respectively. The increasing viscosity ability of PAnBS prepared under the above reaction conditions in sodium chloride or calcium chloride aqueous solution is stronger than that of partially hydrolyzed polyacrylamide with molecular weight of 1.97 ?107and hydrolysis degree of 19.43%. The viscosity of polymer aqueous solution declined slightly with the increase of temperature ,which indicated that the synthesized copolymer had good performance of salt and temperature resistance.

Abstract:A Dendron-jacketed linear polymer is synthesised, ethylenediamine, methacrylate, acrylamide was used in two steps reactions. As the first step, the main chain was prepared by the free radical polymerization reaction of acrylamide and methacrylate, as the second step, the Dendritic side group was introduced to the main chain by the amidation and Michael addition reaction of Ethylenediamine and methacrylate ,thus synthesis a new type Dendron-jacketed linear polymer and the product was characterized by FTIR, the optimized Synthesis conditions as below: reaction temperature 30℃, reaction time 24~48h,reactant malar ratio 1:1. The water-solubility of this product is also evaluated. The result shows that the Dendron-jacketed linear polymer has a remarkable improvement on the anchoring, anti-salts and anti-temperature properties compare to the non-jacketed linear polymer, the molecular structure design achieved the desired result.

Abstract:A new polycarboxylate superplasticizer (FPC) was synthesized by free radical copolymerization of crylic allyl polyoxyethylene ether (APE), acid (AA), sodium methallyl sulfonate (SMAS) and ferulic acid (FA) using ammonium persulfate (APS) as initiator. The optimum FPC was obtained when the molar ratios of APE, AA, SMAS and FA was 1: 5: 0.3: 0.15 using 3% APS by monomers total mass at 85℃ for 4 h. The remarkable feature of FPC is that it has the strong adaptability to mud cement. The application results showed that the fluidity of cement paste can reach to 308 mm, and the initial and final setting time is 430 and 502 min, respectively, and the water reducing ratio is 33.2% when FPC solid dosage is 0.2 wt% and mud content is 10 wt%. The results of SEM and compressive strength showed that FPC can make the hardened cement paste become dense and uniformity result in improving the later strength of hardened cement mortar. Key words: polycarboxylate superplasticizer; ferulic acid; microstructure; compressive strength

Abstract:5-Bromo-7,7-dimethyl-7H-benzo[a]fluorine was prepared from 1-Bromonaphthalene in 63.12% yield. The synthetic process of intermediates 2-(1-naphthalenyl)benzaldehyde, 7-methyl-7H-benzo[c]fluorene and, 7-dimethyl-7H-benzo[c]fluorene were optimized. The optimum conditions were as follows: In the synthesis of 2-(1-naphthalenyl)benzaldehyde, when the amount of catalyst Pd(dppf)Cl2 was 3.0% and reaction temperature 40℃, the yield was 96.8%. In the synthesis of 7-methyl-7H-benzo[c]fluorene, when the amount of catalyst Amberlyst 15 ion-exchange resin was 0.6%, reaction temperature 110℃ and reaction time 4 h, the yield was 95.4%. In the synthesis of 7-dimethyl-7H-benzo[c]fluorene, when n(methyl 4-methylbenzenesulfinate)/n(7-methyl-7H-benzo[c]fluorene)=2.5:1 and reaction temperature 40℃, the yield was 91.0%. The product was characterized with 1HNMR and ESI-MS.

Abstract:Abstract: Preparation of 4-chlorbenzophenone by acylation of benzene with 4-chlorobenzoyl chloride in the presence of FeCl3/ZnCl2 catalyst under pressure was studied. Thus, 157.6 g benzene was mixed with 88.2 g 4-chlorobenzoyl chloride and1.3 g FeCl3/ZnCl2 in a 1L autoclave. The mixture was reacted for 8 h under 0.85×106～1.1×106Pa and 175～185°C to give 93.1g 4-chlorobenzophenone with yield of 86.2% and purity of 99.8%(by HPLC). The effects of pressure, catalyst and ratio of raw materials on the yield were also investigated. The result of our experiments was proved by productive scale up test, in which 175 kg 4-chlorobenzoyl chloride was used as raw material to afford 4-chlorobenzophenone in a molar yield of 82.7%.

Abstract:Four novel amino thiadiazole containing rosin group were synthesized from the starting material of rosin or disproportionated rosin by purification, Diels-Alder addition reaction and cyclization reaction. Their structures were characterized by IR, 1HNMR, MS, and elemental analysis. Bactericidal activity of amino thiadiazole containing rosin group were evaluated by the minimum inhibition concentration. Preliminary results indicated that these compounds display extensive antibacterial activity. Especially compound 5-dehydroabietyl-2-amino-1,3,4-thiadiazole exhibit excellent antibacterial activity against Staphyloccocus aureu and Staphyloccocus epidermidis, their minimum inhibition concentration are 4μg/mL.

Abstract:Abstract:[2,7,12,18-Tetramethyl-3,8-bis ethyl-13,17-dicarboxy ethyl]-porphyrin (II) was directly prepared from hemin in using HCOOH-Fe powder by changing the molar ratio of Fe powder to hemin. The effects of the dostage of Fe powder, temperature, and time on the yield of II were investigated. The results show that the yield of II reaches 97.6% in the molar ratio of Fe powder to hemin 15:1 and the temperature of 120 ℃ and reaction time is 2 h. The target proucts were characterized by means of 1H NMR, MS, UV-vis and IR.

Abstract:Phenoxy acetic acid was prepared by catalytic oxidation reaction, using phenoxyethanol and oxygen as raw materials. HPLC(liquid chromatograph) was used for quantitative analysis, and FT-IR(Infrared absorption spectrum), NMR (nuclear magnetic resonance) and GC-MS(gas chromatography mass spectrometry) were used for qualitative analysis. Effects of Catalysts, solvents, and reaction conditions on reaction results were investigated. The results show that: N-hydroxy phthalimide(NHPI) is an efficient catalyst, and dimethylglyoxime and cobaltous acetate were suitable cocatalysts, and acetonitrile is a suitable solvent. Phenoxyethanol: 0.1mol, the amount of NHPI is 8% of molar weight of phenoxyethanol, the suitable molar ratio of NHPI: dimethylglyoxime : cobaltous acetate =8: 7.5: 1. Under the suitable reaction conditions: 80 ℃, 0.8 MPa O2 for 6h, the yield of phenoxy acetic acid was reached 68.6%. The plausible reaction pathway was proposed based on GC-MS analysis.