Abstract:Polyvinylidene fluoride flat membranes are prepared via TIPS method by using DBP as diluent and DMAc or DOP as mixed diluent at 150℃ and 220℃ repectively. The water flux and structure of membrane prepared under lower and higher temperature are investigated. The result shows that water flux of membrane prepared with 10% DMAc addition at 150℃ is 28% higher than that prepared with DBP as diluent. water flux tends to decrease when the addition of DMAc is above 10%. Water flux of membrane prepared with 10% DOP addition at 220℃ is 62% lower than that prepared with DBP as diluent. At the same time, the structure of membrane is observed and the reason of formation of different structure is explained.

Abstract:A double-hydrophilic diblock copolymer of poly(N-isopropyl acrylamide) -b-poly(N,N-dimethylamino-2-ethyl methacrylate) (PNIPAm-b-PDMAEMA) with well-defined structure and narrow molecular weight distribution (Mw/Mn = 1.27) was synthesized via reversible addition - fragmentation chain transfer (RAFT) polymerization using S-1-dodecyl-S’-(α,α’-dimethyl-α’’-acetic acid) trithiocarbonate (DDATC) and 2,2-azobisisobutyronitrile (AIBN) as chain transfer agent and initiator, respectively. The PNIPAm-b-PDMAEMA was characterized with FT-IR, 1H-NMR and gel permeation chromatography (GPC). The pH and temperature induced micellization of PNIPAm-b-PDMAEMA in the aqueous solution was investigated by transmittance measurement, fluorescence spectroscopy, potentiometric titration and dynamic light scattering (DLS). The copolymer exhibits temperature-responsive micellization in aqueous solution with a lower critical solution temperature (LCST) of 32.3 oC. As raising the temperature over LCST, the PNIPAm block turned to hydrophobic which caused formation of the global micelle composed of PNIPAm core and PDMAEMA shell. The hydrodynamic radius Rh of the micelle measured with DLS about 50 nm and increased with increasing temperautre. The Rh of the micelles increased with increasing temperature. The copolymer exhibits pH-sensitive associate behavior in aqueous solution and the threshold pH value of the pH-induced micellization is about 9.8 at 25 oC. The Rh of the micelle composed of PDMAEMA core and PNIPAm shell is about 31 nm at pH 11.0.

Abstract:Insoluble β-cyclodextrin polymers (β-CDP) were prepared by β-cyclodextrin (β-CD) with 2,4-diisocyanatotoluene(TDI) as crosslinking agent, and the obtained polymers presented good hydrophilicity by tuning the amount of TDI. They were characterized by FT-IR spectroscopy, X-ray diffraction and thermogravimetric analysis, and their solubility in different solvents as well as their swelling capacity in water were measured. The results indicated that the polymerization between β-CD and TDI indeed occurred. In addition, the decomposition temperature shifted about 350℃, the solubility of β-CDP was lower than 0.1% in the organic solvents and the swell capacity was only 0.4mL/g. All these results showed the improved thermostability, chemical stability and mechanical strength. The β-CDP also presented highly catalytic activity for aqueous oxidation of cinnamaldehyde with hydrogen peroxide as oxidant. The yield of benzaldehyde reached 48% and the CDP was reusable. These results demonstrate that the polymer not only reserve the inclusion ability of β-CD but also can be used for organic reactions in aqueous media.

Abstract:A Gemini surfactant with phthalate ester (SHZ16) was prepared from bis [2- (dimethylamino) ethyl] phthalic ester (I) which was obtained by reacting 2-(dimethylamino) ethanol with phthaloyl dichloride and bromohexadecane, yield 83% (based on phthaloyl dichloride) with the purity of 99.2% (two-phase chemical titration analysis).The criticalmicelle concentration (CMC) was found to be 2.02×10-5mol/L by measuring the electrical conductivity of SHZ16, and its surface tension CMC is 41.87mN/m by a drop volume method. Its edition soluble, viscosity, emulsifying property and foaming property were also studied. The results indicated that SHZ16 is better than traditional surfactant sodium dodecyl sulfate (SDS).

Abstract:In order to improve the production of reducing sugar yield from corn stalk by water/ ethanol extraction after steam explosion, the enzymatic hydrolysis process was optimized. With the response surface methodology, the production of reducing sugar yield can reach 672.36mg/g, when the substrate concentration of 53.8g/L, cellulase loading of 53.32FPU/g and reaction time of 60.45h. Compare to untreated and steam exploded corn stalks, the production of reducing sugar yield increased by 179.21% and 37.29%. Chemical compositions of untreated/treated corn stalk were investigated and their structures were also detected by Scanning Electron Microscope (SEM) and X-ray diffraction (XRD). The results showed that: the relative content of cellulose in corn stalk treated by water/ ethanol extraction increased significantly, the relative crystallinity increased, but the changes of structure lead to the cellulase attach on easier.

Abstract:Perilla frutescens (Lamiaceae) is a widespread medicinal plant traditionally used in China to treat several diseases. In order to enlarge the medication parts, the constituents of essential oils which extracted with microwave-assisted hydrodistillation (MAHD), ultrasound-assisted extraction (UAE), and hydrodistillation (HD) from the seeds of Perilla frutescens were analyzed by capillary GC-MS and elucidated based on the standard mass spectral data. 33, 31 and 29 kinds of volatile components were identified respectively. Relative mass fractions of the constituents were determined by area normalization method. The identified relative contents of essential oils were 97.16%, 97.38% and 96.6%, respectively. There were differences among some chemical constituents of three kinds of essential oils. But their main constituents were n-Hexadecanoic acid, (Z,Z,Z)-9,12,15-Octadecatrien-1-ol and pentyl 2-furyl ketone.

Abstract:A series of Cu–zirconia catalysts containing additives (Mn, La) were prepared by coprecipitation and tested for dehydrogenation oxidation from diethanolamine to iminodiacetic acid. The structure and surface properties of the catalysts were characterized by X-ray powder diffraction (XRD), temperature programmed reduction (TPR), N2O titration and N2 adsorption-desorption techniques. The results showed that the addition of Mn could increase the surface area of catalyst from 105 m2?g-1 to 143 m2?g-1and the dispersion degrees of copper species from 36.5% to 53.6%; The addition of La could inhibit Cu particle from growing up and suppress the crystallization of the catalysts; The catalytic performances of the catalysts were greately improved by the addition of Mn and La together. A synergistic effect in La and Mn co-modified Cu/ZrO2 catalyst was suggested.

Abstract:N and Al co-doped TiO2 nanomaterial (N-Al-TiO2) and Al-doped TiO2 material are synthesized through a solid-state reaction route. The textural properties of the samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), ultraviolet visible light spectroscopy (UV-Vis) and X-ray photoelectron spectroscopy (XPS). The photo- degradation properties of puerarin on the materials from irradiating with visible light are investigated. It clearly shows that the microscopic structure of N-Al-TiO2 nanomaterial with crystal anatase phase is a short-rod shape. N atoms as N3- states have been incorporated into the lattice of TiO2 or have been entered into the interstice of TiO2 lattice. Al ions occupy the sites of Ti in crystal lattice by isomorphous replacement. The percent content (%) of atoms such as N, Al, Ti and O in N-Al-TiO2 nanomaterial is 7.8, 3.6, 32.7 and 55.9, respectively. Moreover, the UV-Vis absorption intensity of N-Al-TiO2 nanomaterial is higher rather than that of pure TiO2 and Al-TiO2 materials. Enjoyably, The visible light degradation activity for puerarin is presented as follows as N-Al-TiO2＞TiO2＞Al-TiO2.

Abstract:3-Hydroxy-4-phenyl-2-butanone has a pleasant mild, warm, creamy and sweet aroma, which is widely used in various flavor formulations. Two different methods of preparing 3-hydroxy-4-phenyl-2-butanone were studied starting from (E)-1-phenyl-1-buten-3-one and 4-phenyl-2-butanone respectively. (E)-1-Phenyl-1-buten-3-one was converted to 3-hydroxy-4-phenyl-2-butanone through epoxidation and reduction. The first step reaction used H2O2 as oxidant to give 1-phenyl-1,2-epoxy-3-butanone in 64% yield; 1-phenyl-1,2-epoxy-3-butanone was reduced by HCOOH at the presence of Pd/C to produce 3-hydroxy-4-phenyl-2-butanone in 67% yield. The overall yield was 43%. 4-Phenyl-2-butanone was converted to 3-hydroxy-4-phenyl-2-butanone through the oxidation of the intermediate silyl enol ether. 4-Phenyl-2-butanone reacted with trimethylsilyl iodide at the presence of hexamethyldisilazane to give 4-phenyl-2-buten-2-yl trimethylsilyl ether in 75% yield. The obtained silyl enol ether was oxidized with m-chloroperoxybenzoic acid to give 3-hydoxy-4-phenyl-2-butanone in 71% yield. The overall yield was 53%. The synthetic route starting from (E)-1-phenyl-1-buten-3-one is one more practical route due to easy operation and commercially available cheap reagents although with a little lower overall yield.

Abstract:In this paper, the selective catalytic hydrogenation of p-tert-butyl-α-methyl cinnamaldehyde (PTBMC) to lilial over 5wt.%Pd/C was investigated. Results showed that K2CO3 modification of the catalyst remarkably improved the reaction rate and the selectivity of lilial. The effect of solvent, temperature, pressure and the initial concentration on the reaction was studied. The conversion of PTBMC is 100% and the selectivity of lilial was up to 98.5% under optimal reaction conditions: c (PTBMC) =0.375mol/L, 40 ℃, 0.5MPa.

Abstract:Microwave-assisted ionic liquid dispersive liquid-liquid microextraction was developed for the determination of three P–hydroxybenzoic easters (parabens). High-performance liquid chromatography coupled with UV detector was used for the determination of parabens. Several important parameters influencing the extraction efficiency such as volume of extraction solvent , disperser solvent, microwave time, centrifugation time and salt effect, were investigated. Under the optimized conditions, the enrichment factors(68.3~124.5).and accepted recoveries (55.5~99.2%) were obtained for the extraction of the target analytes .The calibration curve was linear with correlation coefficient ranged from 0.9989 to 0.9991 in the concentration level of 0.1~50 mg/L and the relative standard deviations(RSD, n = 3) were 4.9~5.1%. The limits of detection for three parabens were 0.6~1.2μg/L This method minimized the use of organic solvents and was successfully applied to the extraction of parabens from water solubility cosmetic samples and real water samples.

Abstract:Li1.3Al0.3Ti1.7(PO4)3 pellets sintered with different mole percentage of Li3PO4 were prepared by sol-gel method. The structural identification, surface morphology, electrochemical window, ionic conductivity and activation energy of the sintered pellets were studied by X-ray diffraction, scanning electron microscopy, cyclic voltammetry, and electrochemical impedance spectroscopy. The results show that all the Li1.3Al0.3Ti1.7(PO4)3 pellets sintered with different mole percentage of Li3PO4 have similar X-ray diffraction patterns. The Li1.3Al0.3Ti1.7(PO4)3 pellet sintered with Li3PO4 has lower porosity and is denser than the pellet without Li3PO4. The addition of Li3PO4 has relatively large effect on the porosity and density of the sintered pellet, however has little effect on the electrochemical window of Li1.3Al0.3Ti1.7(PO4)3. Among the Li1.3Al0.3Ti1.7(PO3)4 pellets sintered with different mole percentage of Li3PO4, the one sintered with 1% Li3PO4 shows the activation energy of 0.3142 eV and the highest ionic conductivity of 6.15?10-4 S.cm-1.

Abstract:Cyclodextrin polymers were synthesized by polyaddition cross-linking reaction of cyclodextrin and diphenyl methane diisocyanate.Infrared spectroscopy(IR), Scanning electron microscopy(SEM), Elemental analyzer(EA) techniques were used to characterize the cross-linked polymers. The factors affecting the adoption capacity of the cross-linked polymer on phenol were investigated, the dosage of cross-linked polymer and initial phenol concentration.The results indicate that the cross-linked polymers retained the structure of β-cyclodextrin cavity, surface morphology changed from layer to layered crosslinking and molecular formula was (C42H70O35)7.45. Under the condition of wastewater pH 5-7,temperature30 ℃, mechanical stirring 150 r/min,the removal rate of the phenol was up to 98.5% at using amount of 40mg /mL in 40 min contact time, The removal rate of the phenol is still up to 97%, after 6 times repeated usage.

Abstract:The condensation of ethyl bicyclic phosphite (1-ethyl-4-phospha-3,5,8-trioxabicyclo-[2,2,2]-octane) and dimethyl methylphosphonate has been investigated using self-made ionic liquid [Bmim]BF4 as catalyst under solvent-free conditions. The effects of process parameters, such as molar ratio, reaction temperature and catalyst on the yield were studied respectively from the orthogonal experiment.The suitable synthesis conditions as follows: the molar ratio of ethyl bicyclic phosphite and dimethyl methylphosphonate is 1:1.6,reaction temperature is 185℃,reaction time is 16h,catalyst dosage is 0.4% of the amount of all. The cyclic phosphonate ester was obtained in this condition with the yield 98%. TG test under pure nitrogen showed it had high residual char rate at 500℃.

Abstract:Based on the study of water number, cloud point, surface tension of hyperbranched polyglycerol modified with short oligo(propylene oxide) segments with different structure, the effect of polymer concentration and temperature on the anti-emulsifying behavior of 150SN lubricating base oil is investigated. The results show that HLB (hydrophile-lipophile balance) value, concentration of the polymer significantly affects the anti-emulsifying properties. The HLB value of 14.7~14.9 (water number method) and the cloud point of 58.6°C~65.1°C are favorable for showing better anti-emulsify behavior at the polymer concentration of 2.0×10-2 g/L. Moverover, the anti-emulsifying behavior of these polymers are improved with temperature increasing.

Abstract:The nanoscale phthalocyanine blue dispersion was prepared by emulsion polymerization. The effect of the co-monomer structure, amount of initiator, reaction temperature and time on particle size was investigated. The results showed that styrene was suitable for preparation of encapsulated pigment dispersion, the optimal encapsulation conditions were that the weight ratio of styrene to phthalocyanine blue, initiator APS to St, reaction temperature and reaction time was about 20% , 1.0%, 70~80℃ and 2h respectively. The thermal stability, pH stability and centrifugal stability were improved greatly after emulsion polymerization, FT-IR and TEM showed that some copolymer was coated on the phthalocyanine blue pigment surface, particle size distribution measured by DLS showed that the particle size of encapsulated pigment dispersion was small and uniform.

Abstract:The preparation process of DL-thero-p-methylsulfonylphenylserine ethyl ester, using p-methylsulfonylphenylserine copper as raw material and concentrated sulfuric acid as catalyst, had been studied in this paper. After studying on the factors that influenced on the preparation, the optimal conditions were determined as follows: n(p-methylsulfonylphenylserine copper) : n(concentrated sulfuric acid) : n(ethanol)=1 : 6 : 50, the reaction temperature was 83℃, the reaction time was 10 hours，the crystallization temperature was 0℃ and the value of pH, during the process of DL-thero-p-methylsulfonylphenylserine ethyl ester precipitating from ammonia, was 7.5. The yield of DL-thero-p-methylsulfonylphenylserine ethyl ester was approximately 92% under the optimal conditions. Then the DL-thero-p-methylsulfonylphenylserine ethyl ester was recycled from liquid waste, which were produced during the esterification process and the process of DL-thero-p-methylsulfonylphenylserine ethyl ester precipitating from ammonia. After that, the yield of DL-thero-p-methylsulfonylphenylserine ethyl ester increased to approximately 98%. The products were analysed and characterized by the means of IR, 1H NMR and HPLC. And it was comfirmed that the products were highly purified DL-thero-p-methylsulfonylphenylserine ethyl ester. Chiral separation of DL-thero-p-methylsulfonylphenylserine ethyl ester, using D-tartaric acid as chiral selector,the results demonstrated that the yield of D-thero-p-methylsulfonylphenylserine ethyl ester was 93.81% under the optimal conditions as follows: n (DL-thero-p-methylsulfonylphenylserine ethyl ester) : n (D-tartaric acid) : n (methanol) = 1:1:50, DL-thero-p-methylsulfonylphenylserine ethyl ester precipitated from ammonia when the value of pH was 7.5.

Abstract:The synthetic route of (2R, 3S)-2-amino-3-hydroxysuccinic acid hydrochloride was introduced. It was synthesized via ring forming, ring opening, reduction and hydrolysis reaction, which the D-diethyl tartrate was the starting compound. The total yield of the four steps is 42.04%.

Abstract:2,3,5,6-Tetrachloropyridine (TCP) was prepared by cyclization reaction of 2,2,4-trichloro-4- cyanomethylbutyrate (MTCB) synthesized from methyl trichloroacetate (MTCA) and acrylonitrile (AN). The results of GC/MS showed that the product of cyclization reaction was TCP. The optimum reaction conditions were phosphorus oxychloride and MTCB in molar ratio 2:1, reaction temperature 140℃ and reaction time 4 h. The yield of TCP was 93% under these conditions. Based on works aforementioned, the possible cyclization mechanism of MTCB was discussed.

Abstract:2,6-dimethyl-gamma-pyrone was synthesized via the Claisen condensation with acetylacetone and methyl acetate as raw materials, tetrahydrofuran as solvent, sodium ethylate as catalyst. The qualitative and quantitative analysis was conducted by high performance liquid chromatography(HPLC). Effects of reaction conditions on the properties of 2,6-dimethyl-gamma-pyrone were investigated by single factor experiments. The results showed that the yield of 2,6-dimethyl-gamma-pyrone could reach 13.32% and its content was 95.37% calculated by acetylacetone under the following reaction conditions: the molar ratio of acetylacetone to methyl acetate and sodium ethylate 1.0:2.5:2.0, reaction temperature was 85 ℃, reaction time was 6 hours.

Abstract:The keggin-type H6PMo9V3O40 on silica gel had be prepared and worked very efficiently with high para selectivity for the mononitration of methyl salicylate with nitric acid using carbon tetrachloride as solvent. The effects of various parameters such as time of reaction, temperature, weight of catalyst and nitric acid had been studied. The yield of methyl mononitrosalicylate was up to 94% with p/o 6.58. The catalyst could be recovered easily and reused for fived times with high catalytic activity.

Abstract:Abstract: 2-[2-(4-methoxy-3,5-dimethyl) pyridlmethylthio]-5-methoxyimidazo [4,5-b] pyridine was prepared with 2-chloromethyl-4-methoxy-3,5-dimethyl pyridine hydrochloride (2) and 2-mercapto-5-methoxyimidazo[4,5-b]pyridine (3) in the solution of sodium hydroxide at 30癈,the yield reached 90.1%. Subsequently, the oxidation of sulfide (3) with hydrogen peroxide of the massfraction of 30% afforded the target compound (1), tenatoprazole. The yield reached 86.3% .The overall yield reached 77.8 %.The structure of the product was characterized by IR, 1HNMR,proved the structure of the product was correct .

Abstract:The application performance of ceramic slurry blended with modified sodium lignosulfonate GCL3S was studied, and results showed that GCL3S could obviously improve the dispersion and stability performance of the ceramic slurry. When the addition amount of GCL3S-1 is 0.3%, with the outflow time 41.79 s and thickening degree 1.37, the mass fraction of ceramic slurry could reach 71.26%. With the increase of molecular weight, the performance of ceramic slurry was improved firstly and then decreased. GCL3S-2 with Mw about 27700 had the best dispersion and stability performance of the ceramic slurry. When incorporated with sodium silicate, sodium hexametaphosphate, sodium pyrophosphate and sodium tripolyphosphate respectively, GCL3S-1 could further improve the dispersion performance of ceramic slurry. The outflow time of ceramic slurry was only 38.81 s when the mass ratio of GCL3S-1 to sodium hexametaphosphate was 1:1and the total addition amount was 0.2%. It means that the dispersion performance of this composite dispersant was significantly better than that of common inorganic dispersants.

Abstract:Abstract: To improve anti-light performance of B72, an acrylic resin and extensively used for relic protection，six different hindered amine light stabilizers (HALS) were selected to stabilize B72. From the experiment results, it had been showed that the color of B72 modified with HALS-5060 became yellow obviously in the aging process, even when HALS-5060 adding to B72，and this hindered amine light stabilizer was not suitable to modify B72. The stability of B72 modified with high molecular weight stabilizers, HALS-622 and HALS-944, was better than that of B72 modified with low molecular weight stabilizers, HALS-480, HALS-508 and HALS-292. And the performance of HALS-622 with low alkalinity was more outstanding. Therefore, the lifespan of B72 could be extended by its modification with high molecular weight and low alkaline HALS, which was a new method to conserve cultural heritage effectively.