Abstract:N,N-dimethyl-10H-phenothiazine-2-sulfonamide is the very important intermediate of　 Pipothiazine which is the representative drug of anti-psychotic disorders.In this study, o-bromoaniline was condensed and hydrolysesed , then condensed by N,N-dimethyl-4-chloro-3-nitrobenzenesulfonamide,and reduced by zinc dust,after via Ullmann reaction to give the final target compounds. The effects of different solvent/base、temperature on the yield of condensation,reducing agent proportion on the yield of the reduction,and catalyst agent proportion、reaction temperature and reaction time on the yield of the Ullmann reaction were studied.After 5 steps,the total yield could reach up to 45.5%, the reaction condition was mild,and easily to be treated,the structure of the targer compound was confirmed by means of ESI-MS and 1HNMR.

Abstract:The low-temperature self-crosslinkable acrylate emulsion with core-shell structure was synthesized by semi-continuous seed emulsion polymerization technology, using methyl methacrylate (MMA), butyl acrylate (BA), methacrylic acid (MAA), diacetone acrylamide (DAAM) as comonomers, and characterized by FTIR, TEM and DSC. The results show that the particle size and gel amount increased with w(DAAM). When w(DAAM)= 2%, m(ADH)/m(DAAM)=0.8, the adhesion was up to 90%, water resistant time was up to 150h. FTIR test confirmed that crosslinking reaction between DAAM and ADH could occur when film forming at low temperature. DSC analysis indicated that the glass transition temperature of the film after crosslinking is increased by 5.2℃. The TEM images confirmed spherical latex particles with core-shell structure.

Abstract:A ratiometric fluorescent sensor for Cysteine (Cys) was synthesized based on Diketopyrrolopyrrole and then characterized by 1H-NMR and MS. The maximum emission wavelength located at 576 nm of the sensor displayed a blue-shift to 536 nm induced by Cys and meanwhile, the fluorescence color changed from yellow to green which could be observed through naked eyes. Moreover, DPP-CHO was experimentally proved a specific sensor to Cys without interferences of other amino acids. Whereafter, its utility was carried out to detect Cys quantitatively according to the liner relationship between concentrations of Cys (0～300 μmol/L) and relevant F536/F576 values of the sensor.

Abstract:A method is described for the identification of degradation impurities in Cefodizime solution by ultra performance liquid chromatography and tandem mass spectrometry(UPLC-MS). UPLC-MS method was used to determine the degradation impurities of cefodizime solution at high temperature, acid-base and oxidation conditions. The method identified impurities as anti-form, Δ3-cephem form and degradation impurity based on analysis retention-times, full scan MS and MS2 spectra among extracts , and their content could be increased by heat, acid-base and oxidation. Cefodizime is unstable when exposed to head, acid, alkali and oxygen. Thus, it should be stored in cold, dark and relative humidity below 60%. In addition, the solution should be freshly used.

Abstract:Tyrosine decarboxylase (TDC) is an enzyme that catalyzes the decarboxylation of L-tyrosine to produce tyramine and CO2. In this study, the vector pET-28a was used to recombinant expressed the tdc gene from Lactobacillus brevis in Escherichia coli BL21 (DE3). Several influencing factors of the enzyme reaction, such as pH, temperature, coenzyme, concentration of substrate, were all investigated. The results indicated that the recombinant tyrosine decarboxylase was successfully expressed and the reaction was optimal at pH 5.5 and 40℃, 0.02 g/mL cells, 0.2 M acetic acid buffer solution (pH 5.5), 0.2mM 5-pyridoxal phosphate and 0.18 g/mL L-tyrosine. After 7 hours, the mole conversion rate of L-tyrosine was up to 99%. TDC’s enzyme activity is 29.2 U/g. The Km and Vmax values of TDC were 0.71mM and 9.31mol/L?min?g.

Abstract:With polyoxyethylene polyoxypropylene epoxy ether and polyoxyethylene polyoxypropylene ether as the branched chains,polysiloxane as the based chain,under the isopropyl alcohol solvent,using chloroplatinic acid as the catalyst,through silicon hydrogen addition reaction, synthesized the polyether polysiloxane crude oil demulsifier.Fixed n (epoxy ether) : n (methyl ether) = 1:1, the research shows that n (Si—H) : n (C=C) = 1:1.15, temperature 105 ℃, the reaction time of 5 h, 30 ug/g catalyst and solvent dosage 40% overall (raw material), the conversion rate reached 92.62%, and by FTIR and 1H NMR had been used to characterize the structure of the product, spectra analysis shows that expected product was synthesized. Its critical Angle beam is determined by the surface tensiometer 0.7 g/L, minimum surface tension of 24.2 mN/m. The Demulsifier in demulsification temperature 70 ℃, the amount of 100mg/L, to Yanchang Yongping crude oil dehydration rate reached 88.42%, has good demulsification performance.

Abstract:The anionic conducting membrane material was prepared based on polysulfone in this work. Casting solution of quaternary phosphonium PSF blended with quaternary ammonium polysulfone which exhibits excellent mechanical properties to prepare of a novel kind of anion exchange membrane QAPSFOH / QPPSFOH. The blend membrane can improve the difficult question of quaternary phosphonium PSF to form a membrane. By changing the ratio of the two components can obtain different performance anion exchange membranes. When QAPSF: QPPSF material mol ratio of 1:2, the conductivity of the blend membrane was up to 0.0309 S/cm, tensile strength was up to 775 MPa, thermal decomposition temperature can reach 160℃. The anion exchange membrane have been met the requirements of the theory.

Abstract:The supported Nb/USY catalyst with molecular sieve USY as support and niobium acid as Nb source was synthesized by the method of impregnation. The samples were characterized by means of XRD, FT-IR TG-DTA. Using H2O2 as oxidant and Thiophene of isooctane solution as the simulated oil to do experiment. The effects of Nb-Ioading, caIcination temperature and time on the cataIyst activity and the performance of the catalyst regeneration were studied. Through analyzing of the oxidation product, explore the mechanism of oxidative desulfurization. The experimental results indicated that,when the amount of niobic acid loading is 15%, caIcination temperature is 300℃, time is 120min, Nb/USY exhibited the highest activity,in addtion, its regeneration properties were good, the final oxidation product of Thiophene is sulfate.

Abstract:2-Hydroxy-4-acryloy benzophenone(HAB) was synthesized from acrylicchloride and 2,4-dihydroxybenzophenone(UV-0). Poly(HAB-OAIG)(PHIG) was prepared by polymerization of HAB with 3-O-acryloyl-1,2,5,6-di-O-isopropynylene-α-D-glucose(OAIG). Then, the copolymer poly(HAB-co-3-O-acryloyl-α-D-glucose)(PHG) was obtained by hydrolysis of PHIG via trifluoroacetic acid. These structures were characterized mainly by FTIR, 1HNMR and GPC. The UV-Vis spectroscopies revealed that PHG is of good ultraviolet absorption ability in the wavelength range of 280-360 nm, and the maximum absorption wavelength is 331 nm. MTT experiments showed the relative cell proliferation rate of L929 cells which were treated with different concentrations extracts of PHG is greater than 80%. And with the concentration increases, the relative appreciation rate was not significantly reduced. These data demonstrated that PHG has good biocompatibility.

Abstract:A complex [Cu(4-Me-SA)(Phen)]•2H2O, (Phen = 1,10-phenanthroline and 4-Me-SA = 4-methyl salicylate has been synthesized from solvothermal reaction and characterized by single crystal X-ray diffraction analysis, studied by element analysis, infrared spectrum, UV-spectrum, thermogravimetric analysis and fluorescence spectrophotometer(FS), respectively. The result shows that the crystal structure belongs to monoclinic, space group P2(1)/c with a = 0.8324(3) nm, b = 1.2644(5) nm, c = 1.7493(7) nm, α = 90.00°, β = 100.404(7)°, γ = 90.00°, V = 1810.8(12) nm3, and Z = 4. The Cu atom is four-coordinated by two oxygen atoms from one 4-methyl salicylate and two nitrogen atoms from one 1,10-phenanthroline. Hydrogen bonds and aromatic π-π stacking interactions assemble the title complex into a stable three dimensional network. Luminescence measuremet shows that the complex has fluorescent property.

Abstract:The silicone oil/water emulsion was prepared by high-speed shear emulsification method with dimethicone（1000 mPa•s）as the main material, nonionic surfactant NP-4 and Tween-80 as emulsifier, gelatin as stabilizer. The preparation conditions effecting on performances of silicone oil emulsion were discussed, such as HLB value, the amount of emulsifier, the amount of silicone oil, the amount of stabilizer, emulsification temperature, shear speed，shear time, etc. The optimal process conditions for preparing silicone oil emulsion were identified as follows: in the emulsion systems, w(silicone oil)=35%, w(emulsifier)=10.5% and w(stabilizer)= 0.3%; the emulsification temperature was 35℃, the shear speed was 11000 r/min and the shear time was 10 min. Under these conditions, the obtained silicone oil emulsion was white, fine and homogeneous liquid, and had good dispersibility and stability. The average particle diameter was about 1.2μm, and the solid content of emulsion was about 46%.

Abstract:Enzymatic polymerization of catechol was conducted using laccase enzyme in Sodium Dodecylbenzenesulfonate Micellar Solutions. The influence of temperature, pH value, the molar ratio of catechol to SDBS and catechol concentration on polymerization were studied. FT-IR, GPC, DSC and TGA were employed to characterize the synthesized poly(catechol). The results showed that the optimum reaction conditions were as follows: the temperatures was 40℃, pH value of the reaction was 5.5, the concentration of SDBS was 2.5 mmol/L and the molar ratio of catechol to SDBS was 2:1. The number average molecular weight of poly(catechol) was found as 810Da. Thermal analysis showed that the polymer glass transition temperature was 95 ℃.

Abstract:In order to achieve the highly-effective gas-phase selective oxidation of alcohols, the gold catalyst was prepared using Mn3O4-modified SiO2 as support, and the modification conditions of support, the preparation and reaction conditions of catalyst were investigated. The results showed that benzyl alcohol conversion and benzaldehyde selectivity were enhanced over the modified catalyst. For example, benzyl alcohol conversion of 96% and benzaldehyde selectivity of 98% could be achieved at 250℃. The catalysts were characterized by X-ray diffraction (XRD) and transmission electron microscope (TEM), and the results showed that the Mn3O4 was dispersed in the form of monolayer. Gold particle size is 12-14 nm, but exhibits excellent performance for the alcohol oxidation due to the Au-Mn3O4 interaction.

Abstract:TiO2 coated with CdS (CdS/TiO2) composite nanoparticles were prepared by chemical precipitation method. They were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and UV-vis diffuse reflection absorption spectra. The activity of sample was explored with photocatalytic hydrogen evolution under visible light irradiation as a probe reaction. The results showed that the particle size of composite nanoparticles was about 40nm. TiO2 and CdS in the composites could be indexed to an anatase phase and hexagonal crystal, respectively. The absorption edge of composites showed an obvious red-shift and absorption peak was appeared in the visible light region. The experimental of photocatalytic hydrogen generation showed that the composites had high activity of hydrogen generation and stability.

Abstract:The synthetic technique of TG101209 for treating bone marrow hyperplastic tumor was studied.2-Chloro-4-amino-5-methyl-pyrimidine(B) was prepared by chlorination and substitution reaction of 2,4-dihydroxy-5-methylpyrimidinnel, phosphorus oxychloride and ammonium hydroxide.B reacted with 3-bromo-N-t-butyl benzenesulfonic amide (C) to give 3-[(2-chloro-5-methyl-4-pyrimidinyl) amino]-N-t-butylbenzenesulfonic amide (D) by Buchwald coupling reaction.D reacted with CH3OH-HCl in the methanol to afford 3- [(2-chloro-5-methyl-4-pyrimidinyl) amino]-N-tert-butylbenzenesuiphonamide hydrochloride (E). (N-tert-butyl-3-(5-methyl-2-[4-(4-methyl-1-piperazinyl)-phenylamino]-pyrimidine-4-ylamino)-benzenesulfonamide)(TG101209) was synthesized by nucleophilic substitution reaction of the intermediate (E) and 1-methyl-4-(4-aminophenyl)piperidine (G). The overall yield was 30.9%. HPLC purity was 99.7%. (N-tert-butyl-3-(5-methyl-2-[4-(4-methyl-1-piperazinyl)-phenylamino]-pyrimidin-4-ylamino)-benzenesulfonamide)(TG101209) was synthesized by nucleophilic substitution reaction of the intermediate (E) and (G).The overall yield was 30.9%.HPLC purity is 99.7%.

Abstract:The composite PAA/PVP/PGS(PAPP) was prepared by free radical polymerization using N, N'-methylenebisacrylamide (MBA) as the cross-linking agent, potassium persulfate (KPS) as the initiator, acrylic acid (AA), polyvinylpyrrolidone (PVP) and palygorskite (PGS) as the raw material. Orthogonal experiments were designed to optimize the proportion of each raw material. The morphology and structure were characterized by scanning electron microscopy (SEM) and Fourier Transform Infrared spectrometer (FT-IR). The results showed that the graft copolymerization reaction was taken placed between acrylic acid and palygorskite micropowder, the clay in composite material dispersed well. The adsorption study showed that the composite have a good adsorption capacity for methyl blue solution, and it’s adsorption capacity could reached 968.69 mg/g. Therefore, It can be used as a potential adsorbent for the removal of anionic dyes from wastewater .

Abstract:Nanometer titania has been prepared by hydrolysis of titanium(Ⅳ) sulfate(Ti(SO4)2), and the product was characterized by XRD, SEM and BET. Effects of synthesis methods, titanium(Ⅳ) sulfate concentration, hydrolysis temperature, desiccation temperature, addition of dispersant PVA and strring on adsorption behavior of TiO2 were investigated，and the optimum TiO2 synthesized condition was obtained. In addition, influences of pH value of As(Ⅴ)solution, adsorption kinetics and initial As(Ⅴ)concentration on arsenate adsorption by TiO2 were studied. Results suggested that adsorption capacity of As(Ⅴ) by TiO2 approached 89.28mg•g-1 at the condition of 80℃hydrolysis temperature, 100℃desiccation temperature, 0.2mol/L titanium(Ⅳ) sulfate concentration, pH 6.0 and 100mg•L -1As(Ⅴ)initial concentration. It was found that anatase nanometer tatania was formed by XRD, the mean particle size of nanocrystalline TiO2 was less than 20nm by SEM, and the specific surface area was 167 m2/g by BET.

Abstract:Cationic poly(amide-ester) (PAE-GTAC) was synthesized from dendritic poly(amine-ester)[PAE(NH2)8] and glycidyl trimethyl ammonium chloride(GTAC). The effects of reaction temperature, reaction time and the mole ratio of reactants on the product yield were studied through orthogonal experiments. The PAE-GTAC structure was identified by means of FTIR and NMR. The effects of the amount of PAE-GTAC , centrifugation time and pH on the removal of Cr3 and dyes(methyl orange、titan yellow and xylenol orange )were discussed. Under the optimum conditions: reaction temperature 45 ℃，reaction time 5 h and n(PAE(NH2)8)∶n(GTAC)= 1:16，isopropanol as solvent, the yield of PAE-GTAC was 66.28%. At 25℃, pH=8.87, a rotational speed of 3000 r/min for centrifugation 13min with 25mL PAE-GTAC (c=0.01 mol/L) was treated 10mL CrCl3 (c=0.1mol/L) solution, the highest removal rate was 97.56%; at 25℃, pH=1.51、2.03 and 1.52, after oscillated 15min, a rotational speed of 3000 r/min for centrifugation 10min with 25mL PAE-GTAC (c=0.01 mol/L) was treated 10mL dyes (c=1.2?0-5 mol/L) solution, the highest removal rate of methyl orange, titan yellow and xylenol orange was 84.16%、92.25% and 97.35% respectively.

Abstract:Under the catalysis of chloroplatinic acid，a polysiloxane heavy oil demulsifier，was synthesized taking methyl terminated polyether，the self-made low hydrogen silicone oil and acrylic nonylphenol polyoxyethylene polyoxypropylene ester as raw materials.The chemical structure were characterized by IR spectroscopy and nuclear magnetic resonance (1HNMR) spectrum．On basis of the single factor test the effects of different factors on the conversion rate of reation，to determine the optimum technological conditions as follows：the reaction temperature was 95 ℃，the reaction time was 7 h，the molar ratio of silicon-hydrogen bonds was 1.0:1.2，the amount of catalyst was 40 μg/g．Under this condition，the conversion rate of reation reached 92.86%.The performance tests show that the synthesized crude oil demulsifier with the optimal conditions exerted better effects．

Abstract:A new maleate was synthesized by polypropylene glycol and maleic anhydride under the condition that using p-toluene sulfonic acid as catalyzer . And then an oil-soluble terpolymer was synthesized by vinyl acetate, acrylamide and the maleate which was prepared before. The chemical structure of the copolymer was identified by IR spectrometric data. The optimum reaction conditions were obtained as follows : the monomer molar ratio of vinyl acetate, acrylamide and maleate was 6:2:1, with initiator dosage of 0.9%, polymerization temperature of 75℃and reaction time of 6 hours. The viscosity was decreased from 3790mPa•s to 1110mPa•s when the dosage of viscosity reducer was 600mg/L at 50℃.

Abstract:Acrylic acid-itaconic acid copolymers were synthesized in water. Ammonium persulfate was used as initiator and sodium hypophosphite as chain transfer agent. The influence of different reaction conditions on the clay slurry viscosity was investigated. The optimal conditions were shown as follow: the temperature was 80℃, 0.8% ammonium persulfate by the mass of monomer, 9% sodium hypophosphite, and 0.9% initiator. The structure of copolymer was characterized by FTIR. The viscosity and bending strength of the slurry and the microstructure of the fracture surface were also studied. The results showed when adding 0.25% copolymer, the viscosity of the clay slurry was reduced from 1998mPa•s to 690mPa•s and the body strength was increased from 1.96MPa to 2.88MPa.

Abstract:The ceramic body slurry's viscosity are determined to characterize the dispersion property of ceramic body slurry with two self-made polycarboxylate superplasticizer of different molecular structures. The experiment of static adsorption studied kinetic study about adsorption of two self-made polycarboxylate superplasticizer using ceramic blank. The test data were further analyzed with pseudo-second order kinetics. The results show that the dispersion property of polycarboxylate superplasticizer of linear MA/AA/AMPS is much better than that of comb AMPS-modified polyacrylic acid superplasticizer in the ceramic body slurry. The saturation amount of polycarboxylate superplasticizer of linear MA/AA/AMPS adsorbed onto ceramic blank is more than 2 times that of comb AMPS-modified polyacrylic acid superplasticizer. The pseudo-second order kinetic equation was found to best-fit the test data as judged by the correlation coefficients.

Abstract:In this article，four kinds of different alkyl substituted diallylmethyl quaternary ammonium salt monomers were synthesized. Four kinds of diallylmethylalkyl (C3, C5, C7, C9) quaternary ammonium salts were synthesized using diallylmethylamine and 1-bromide straight chain alkanes as raw materials.The effects of reaction on time，temperature，molar ratio of raw materials and different solvents were discussed. Structures of the products were characterized by IR，1HNMR and 13CNMR. The results showed that the yields of the products were 78.18%，82.54%，84.63% and 81.32%，respectivly,under the optimum synthetic conditions. The obtained products possessed the expected structures. In addition，the products were miscible well with polar solvent and their melting points decreased with the increase of the straight alkyl chain length. The progresses completed above had provided a foundation for the researches on preparation，mechanism and application of the corresponding polymers.

Abstract:Using homogeneous pump, and by controlling the reaction temperature in stages, dimethyl diallyl ammonium chloride (DMDAAC) monomer was synthesized in one step using dimethy lamine, allyl chloride and liquid caustic soda as starting materials. In the vacuum distillation purification process, the pH value of the crude DMDAAC solution was adjusted via a syringe pump adding liquid caustic soda. The results showed that the use of homogeneous pump improved the materials mixing, shortened the dropping time of allyl chloride from 5h to 3.5h, and prevented the occurrence of side reactions. The yield is up to 91.5%, which is 21.11% higher than that in the traditional one-step method. And the polymerization performance is also studied. Molecular weight of homopolymer can reach to 125,000. The intrinsic viscosity of the polymer product increased from the original value 1.19 dl•g-1 to 2.80 dl•g-1. The monomer conversion rate increased from 90.08 % to 99.23 %. The 20 L bench-scale research for this technology have been done.

Abstract:K2CO3 was utilized as an friendly catalyst for the environmentally fast and simple synthesis of ten 3-substituted coumarin derivatives by the Knoevenagel condensation of salicylaldehyde and its derivatives with diethyl malonate, ethyl acetoaceate or methyl acetoaceate under solvent free conditions. Three effect on the yield of coumarin-3-ethyl formate was investigated. The results showed that coumarin-3-ethyl formate were obtained 88.1% yields within based on 20 mmol of salicylaldehyde, molar ratio of salicylaldehyde to diethyl malonate 1︰1.2, dosage of K2CO3 0.1 mmol and time of reaction 15-18 min. When ethyl (or methyl) acetoaceate displaces diethyl malonate, 3-acetyl coumarin were synthesized with the yield 84.7%(or 82.9%). When solid substituted salicylaldehyde displaces salicylaldehyde with diethyl malonate, ethyl (or methyl) acetoacetate at a mole ratio of 1︰2.0, eight 3-substituted coumarin derivatives were synthesized with the yield from 62.5%~89.0%(or 58.1%~83.0%), the electron donating groups substituted on salicylaldehyde, such as diethyl amino-group, was favorable to the condensation reaction. Key words: Knoevenagel condensation; 3-Substituted Coumarins; salicylaldehyde and its derivatives; Reactive methylene compound; K2CO3; solvent-free synthesis