Abstract:The physical and chemical properties of Tetracalcium phosphate (TTCP) +Monocalcium phosphate monohydrate (MCPM) +β-Tricalaium phosphate (β-TCP) bone cements with polyacrylic acid (PAA) hardening liquid have been studied. The results showed that the increasing of the liquid to powder ratio caused an increase in the setting time of cements which allows the possibility for their control, the final setting time was 7min when the liquid to powder ratio was 1.0; Compressive strength was also influenced by the liquid to powder ratio, when the liquid to powder ratio was 0.8, it reached the maximum 20.86 MPa. The degradation rate guadully increased along increasing immersion time, then attained stable. From XRD phase analysis, it was found that Hydroxyapatite (HA) and Dicalcium phosphate dihydrate (DCPD) were created in the setting process, suggesting that the various crystal phase in bone cement resulted in different degradation rate.

Abstract:Li1.3Al0.3Ti1.7(PO4)3-coated LiMn2O4 was prepared by wet chemical route. The phase, surface morphology, and electrochemical properties of the prepared powders were characterized by X-ray diffraction, scanning electron micrograph, and galvanostatic charge-discharge experiments. Li1.3Al0.3Ti1.7(PO4)3-coated LiMn2O4 has similar X-ray diffraction patterns, cyclic voltammograms, and charge-transfer resistance as LiMn2O4. The two powders show similar values of lithium-ion diffusion coefficient. When cycled at room temperature and 55癈 for 40 times at the charge-discharge rate of 0.2C, Li1.3Al0.3Ti1.7(PO4)3-coated LiMn2O4 shows capacity retention of 98.2% and 93.9%, respectively, which are considerably higher than the values of 85.4% and 79.1 % for the uncoated one. Both the capacity retention difference between LATP-coated LiMn2O4 and LiMn2O4 cycling at room temperature and 55癈 become larger with the increase of the charge-discharge rate. When the charge-discharge reaches 2C, the capacity retention of LATP-coated LiMn2O4 becomes 8.4% higher than uncoated LiMn2O4 for room temperature cycling, and it becomes 11.1% higher than the latter when cycled at 55癈.

Abstract:In this paper, the composite self-assembled super-hydrophobic film was prepared on copper surface with (3-mercaptopropyl)trimethoxysilane(MPTS) and octyltriethoxysilane(OS). The copper surface was etched in HNO3 (6.5 wt.%) solution before coated. The structure of composite film was analyzed by Fourier transform infrared spectra. Scanning electronic microscopy (SEM) indicated that the film had nano-micro scale structure. The contact angle reached 158.6°with sliding angle 3°, which suggested that the film was super-hydrophobic. The result of salt solution immersion test showed that anti-corrosion property of copper surface was greatly improved.

Abstract:The inclusion complex of methyl methacrylate（MMA） with randomly methylated β-cyclodextrin (RAMEB) was synthesized by solvent method and characterized by TG-DSC, UV．Molar ratio method shows that the 1∶1 inclusion compound has formed between RAMEB and MMA. TG –DSC analysis shows that RAMEB and MMA have formed steady inclusion and the stability of MMA has increased remarkably. Using MMA as monomer, K2S2O8 as initiator, we investigated the influence of RAMEB on the sope-free emulsion polymerization of MMA. It is found that when the addition of RAMEB is 0.5g, the conversion of MMA reached 89.21% in 30min at 75℃. Compared to no addition of RAMEB, the conversion increased 30.6%. When the addition of RAMEB is 1g, the polymerization speed decelerated and monomer conversion was almost the same compared to no addition of RAMEB. The addition of RAMEB increased particle size of PMMA. With the increase of RAMEB, PMMA particles are getting more and more uniform.

Abstract:Starch octanoate (St-C8) with different degree of substitution (DS) were synthesized by corn starch and octanoyl chloride in organic solvent. The structure of St-C8 was identified by infrared spectrum. Moreover, St-C8 was used as the emulsifier of soybean oil and water system. The effect of DS, emulsifier concentration and the proportion of oil phase and water phase (VO/W) on the emulsibility and emulsified stability of emulsion were also investigated in detail. The result indicated that St-C8 exhibited the best emulsibility and emulsified stability when the DS and concentration are 0.37 and 7%, respectively. Furthermore, the emulsion exhibited the best emulsibility and emulsified stability when the VO/W is 4/6 and 2/8, respectively.

Abstract:Allyl polyoxyethylene glycidol ether(APGE) was synthesized with allyl polyoxyethylene ether, epichlorohydrin and sodium hydroxide solution as raw material through two-step method. Polyoxyethylene glycidol ether trisiloxane (PGETS) was prepared by the hydrosilylation from 1,1,1,3,5,5,5-heptamethyltrisiloxane(MDHM) and APGE; and then further underwent a ring-opening reaction with trimethylamine hydrochlorate to form quaternary ammonium salt polyoxyethylene ether trisiloxane surfactant (QASPETSS). The chemical structure of QASPETSS was characterized by IR and 1HNMR. The interfacial properties of QASPETSS were studied by the measurement of equilibrium surface tension in its aqueous solution. Experimental results showed as follows: In the critical micelle concentration of 6.3×10-4mol•L-1, the surface tension of QASPETSS aqueous solution reduced to approximately 22.4 mN•m-1. The saturated adsorption, single QASPETSS average areas on the saturated absorption layer and the micellization standard free energies are 3.6×10-6mol•m-2, 0.46 nm2 and -28.2 kJ•mol-1, respectively.

Abstract:Taking the extraction efficiency of Chrysanthemum morifolium Ramat flavor concret as the index，the L9（34） orthogonal experimentwas applied to optimize．The volatile compositions in the perfume were prepared with simultaneous distillation and extraction equipment (SDE)．They were isolated and indentified by capillary GC-MS method．The optimal extraction conditmns were obtained as followed：φ (alcohol) = 70％，ultrasonic power 800W and time 30 min．88 peaks compounds were isolated and identified. The relative contents of the total peak area were determined by area normalization method. The main volatile compositions were: (+)-Aromadendrene（9.38%）、n-Hexadecanoic acid（5.11%）、β- Panasinsene（4.63%）、Longifolenaldehyde（4.36%）、α-Cedrene oxide（3.97%）、Eudesma-4(14),11-diene（3.67%）、Isoaromadendrene epoxide（3.35%）、1-Fluoro-2-[(Z)-2-methoxyethenyl]benzene（3.17%）、α-Ylangene（3.15%）、Linolic acid（2.68%）、Alloaromadendren（2.54%）、α-Cyperone（2.35%），etc．The optimum process increased the extraction efficiency of Chrysanthemum morifolium Ramat flavor concret．

Abstract:The three-dimensionally layered silicate AMH-3 was obtained in the absence of titanium using silica sol as silica source. Focused on the system, the effect of different synthesis conditions were investigated, and the physicochemical properties of the materials obtained were characterization by XRD, SEM and TG-DSC methods. It was confirmed that the silica source is critical for the formation of AMH-3, the molar ratios of Na2O/SrO and SiO2/SrO also play important roles on synthesis of AMH-3, the results of XRD and TG-DSC analyses indicate that the framework structure is intact after calcination at 450℃.

Abstract:Ａ series of　 Cu2+-substituted composite metal oxides LaMnO3 were prepared by improved amorphous citric precursor method(IACP)， characterized by XRD ,IR,BET and SCM , tested the performance of ethanol to n-butanol and n-butanal without oxygen. The results showed that the Cu2+-substituted products could reserve the perovskite-type crystal structure, and crystalline phases of CuO, MnO2 and La2O3 appeared when the amount of copper increased. The aberrations of B-substituted crystal structure was larger than that A -substituted ,and B-subsituted oxides which showed better activity than the A-subsituted. Among all the catalysts, LaCu0.3Mn0.7O3 exhibited the highest catalytic activity. Under the tempereture of 500℃, the conversation of ethanol was 55.18%, and the selectivity of n-butanal and n-butanol was 41.30% and 24.09%, respectively.

Abstract:The ZB-2 alkali anion exchange fiber column separating and purifying capsaicinoids from capsicum was investigated in the experiment. Through analyzing the SEM before and after the absorption of capsaicinoids by ion exchange fiber, its absorptive ability was determined. And the absorbed compound was capsaicinoids through analyzing the infrared spectrum. Then the relation between the pH, the mass concentration, the flow velocity and the absorptive capacity was investigated. Furthermore, the relation between the ethanol volume score, the flow velocity, the ethanol volume and the desorptive speed was discussed. Then the optimum technology condition was obtained. Under the condition, the capsaicinoids content enhanced from 4.5 % to 92.0 %, and the yield reached 72.3 %. The result indicates that the ion exchange fiber can separate and purify capsaicinoids.

Abstract:Using Leucine and 2,5- hexanedione via Paal-Knorr reaction to form N-(2,5-Dimethyl Pyrrole)-leucine. Then by using DCC as dehydration reagent, DMAP as catalyst, the pyrrole acid derivatives were esterified with different hydroxyl compounds to give new pyrrole esters. The structures of all the compounds were confirmed by IR, 1H NMR, 13C NMR, HRMS spectral analysis. The thermal cracking behavior of pyrrole ester was respectively studied at 300℃、600℃ and 900℃, and 50 kinds of thermolytic products containing various aromas were authenticated which can improve the tobacco’s taste and flavor.

Abstract:4,5-bis(2-bromo-4,5-dihydroxy-benzyl)-1,2-benzenediol Ⅵ was synthesized from veratraldehyde Ⅰ, by employing bromination, reduction, Friedel-Crafts alkylation and demethylation with an overall yield of 53.5%. The structure of compound Ⅵ was elucidated by spectrum techniques including 1H-NMR,13C-NMR and HREIMS. Inhibitory activities of compound Ⅵ and 4,5-bis(2-Bromo-4,5-dimethoxy-benzyl)-1,2-dimethoxybenzene Ⅴ against protein tyrosine phosphatase 1B (PTP1B) were tested by colorimetric assay. Inhibition rates of compound Ⅴ and Ⅵ against PTP1B were 25.08% and 79.48% at 20 mg•L-1, respectively, which indicated that compound Ⅵ was an potential therapeutic agent for treatment of type 2 diabetes mellitus.

Abstract:The synthetic method of a new antithrombotic drug-prasugrel was introduced in this paper. The precursor(Ⅹ) of condensation reaction was synthesized via four steps from 4,5,6,7-tetrahydrothieno[3,2-c]pyridine hydrochloride. Another precursor (Ⅻ) of condensation reaction was synthesized via two steps from 1-(bromomethyl)-2-fluoro benzene. The target product was prepared via condensation, hydrolysis and acetylatio n reactions from the two the precursors. The yield of all synthetic steps is 34.6%. The partly intermediate product and target product was identified by 1H NMR and MS. The synthetic process, featured with simple operations、high yield and easy purification, is not less than the synthetic routes reported by other papers.

Abstract:In order to expand the scope of application of shellac wax, nano-shellac-wax emulsions was prepared by Shah method through single factor experiment to choose factors and levels. Average particle size of the emulsion were optimized through response surface method with three factors and three levels based on principle of Box-behnken design. Results showed that the optimum average particle, the rate of mixing emulsifying temperature are 30.5nm, 15.9%, 890r/min, 90℃, respectively. The particle size, distribution and stability of shellac-wax emulsions are studied with the laser granularity analyzer.The average particle size of shellac-wax emulsions are below 50nm and were well-distributed.

Abstract:The copolymer of p-hydroxybenzaldehyde (PHB) and 4-phenolsuflonate (PHS) was synthesized using horseradish peroxidase (HRP)/H2O2 as catalyst. Firstly, PHB can react with ethylene glycol to generate p-hydroxybenzaldehyde ethylene acetal (PHBEA) so as to protect aldehyde group. Then copolymer of PHBEA and PHS was prepared by enzymatic catalytic polymerization. Finally, the copolymer of PHB-PHS was obtained by getting rid of the aldolization. Effects of monomers composition, system pH, polymerization temperature, amount of HRP and H2O2 dropwise time on copolymerization were investigated. The structure and properties of the copolymer were characterized by FTIR, NMR and GPC. The applied results show that the shrinkage temperature (Ts) of tanned leather may increase from 54°C to 74.5°C, and the copolymer has assisting dyeing and tanning effect on skin fibers.

Abstract:Adsorption properties of cationic dye methylene blue (MB) onto poly (acrylic acid-co-acrylamide)/ attapulgite composite clay were investigated. The effects of various experimental parameters such as pH, concentration of the dye, temperature, contact time, adsorbent dosage, ionic strength and surfactant on adsorption process have been studied. Equilibrium isotherms for the adsorption of the dye were measured experimentally. Results were analyzed by Langmiur and Freundlich equation at different temperatures and the characteristic parameters for the adsorption isotherm were determined. The adsorption process has been found endothermic for MB in nature. The thermodynamic parameters such as Gibbs free energy, change in enthalpy and change in entropy have been calculated. The maximum adsorption capacity for MB was obtained as 1273.3 mg g-1 at the temperature of 60℃. It was observed that the kinetic data fitted well with a pseudo second-order equation. The results showed that the composite attapulgite clay could be employed as low-cost alternatives to traditional agent in wastewater treatment for the removal of color.

Abstract:Phthalate was synthesized via the esterification by phthalic anhydride with aliphatic alcohols when sodium hydrogen sulfate was used as the catalyst. The effects of the length of aliphatic alcohols, types of aliphatic alcohols and content of branched-chain aliphatic alcohol on the properties of phthalate were studied systematically, which can offer the effective theoretical foundation for synthesis of high performance lubricants. Results showed that viscosity and viscosity index of phthalates increased, but their pour point and flash point reduced with an increaseof the length of aliphatic alcohols. For phthalate prepared from aliphatic monohydric alcohol with same carbon atom number, these branched-chain esters had higher viscosity, pour point, flash point, and lower viscosity index than these straight-chain esters. The synthetic esters formed by reacting phthalic anhydride with a mixture of linear and branched aliphatic monohydric alcohol showed properties: high viscosity, low viscosity index, good high-temperature behavior and worse low-temperature behavior. The increase of the branched-chain aliphatic alcohol led to higher viscosity, lower viscosity index. And the pour point and flash point showed serrated variation along with it.

Abstract:A facile synthesis of a novel side-chain sulfonated diamine is developed. The sulfonated diamine was synthesized through two-step reactions, namely the nucleophilic substitution reaction of 2-naphthol-3,6-disulfonic acid sodium salt to 2,4-dinitrofluorobenzene followed by the reduction under SnCl2/HCl system, which gave an overall yield of 32%. The product was characterized by IR and 1H-NMR measurements. The reaction conditions of nucleophilic substitution were investigated, the results showed that the room temperature was prefer to obtain the the sulfonated dinitro intermidate with high purity of 98% and yield of 64%.

Abstract:M-nitrobenzyl bromide and 1-(dibromomethyl)-3-nitrobenzene, which were prepared with m-nitrotoluene, hydrogen peroxide and hydrobromic acid over AIBN, was oxided and hydrolyzed to produce m-nitrobenzaldehyde. Factors influencing bromination, hydrolysis and oxidization were studied. Under the optimal bromination conditions: bromonation temperature 60 ℃, bromination time 4 h, n(m-nitrotoluene) : n(HBr) : n(H2O2) 1:2.5:2.5, the amount of AIBN 0.8 g. Under the optimal oxidization and hydrolysis conditions: oxidization temperature 105 ℃, heat preservation time 8 h, hydrolysis temperature 60 ℃, hydrolysis time 1 h. The yield of m-nitrobenzaldehyde is 58.6%. Purity of product reaches 99.1%. The structure of the product was identified by IR and 1HNMR.

Abstract:The preparation process for o-ethoxy benzoic acid, a key intermediate for sildenafil, was improved with methylsalicylate. Sodium salt of methylsalicylate was firstly prepared and treated with ethyl bromide to give methyl o-ethoxybenzoate, which was hydrolyzed to afford o-ethoxy benzoic acid (HPLC purity 99.88%). The overall yield was 89.5% and It has been produced in Chongqing Kangerwei phamaceutical Co. Ltd.

Abstract:A effective carbonylation of aromatic nitro-compounds with thiols or thiophenols catalyzed by Pd-Fe/TiO2 in ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim]PF6) was studied. The influences of reaction medium, Pd and Fe loading, molar ratio of nitro-compound to thiols, catalyst dosage and reaction temperature on the carbonylation reactions were investigated. Pd-Fe/TiO2 catalyst with mass fraction of Pd 0.5% and mass fraction of Fe 0.3% exhibits high activity for carbonylation reactions. The carbonylation of some aromatic nitro-compounds with thiols or thiophenols catalyzed by Pd-Fe/TiO2 in ionic liquid can proceed well to thiocarbamates in good yield under the conditions of nitro-compound 10 mmol, thiols or thiophenols 11 mmol, catalyst dosage 36 mg, ionic liquid 10 mL, CO pressure 0.1 MPa, reaction temperature 30 ℃, reaction time 3～8 h. The catalyst and ionic liquid can be reused for six times without significant decrease in the yield of thiocarbamates.

Abstract:N-Phenylpyrrolidine is synthesized from aniline and 1,4-butanediol dimethanesulfonate by microwave-assisted reaction in the presence of deacid reagent. Through single factor and orthogonal experiments, various factors influencing the yield are investigated. The optimal reaction conditions are obtained as follows: n(aniline) : n(1,4-butanediol dimethanesulfonate): n(potassium carbonate) = 1:1.3:1.3, reaction time 60 minutes, microwave power 200 W, reaction temperature 100 ℃, the yield 78.6 % of N-phenylpyrrolidine can be achieved in water under this condition. The optimal process conditions have advantages of rapid reaction, mild conditions, simple operation, high product purity, and environment-friendliness. So it is suitable for industrialized production.

Abstract:protoporhyrin(2) was prepared by the demetalation reaction of hemin using HCOOH-Fe powder in formic acid. And [2, 7, 12, 18-tetramethyl-3, 8-bis (-1-hydroxy ethyl)-13, 17-dicarboxy ethyl]-porphyrin (hemato- porphyrin) was prepared through a “one pot” reaction of a HBr-acetic acid addition reaction and a OH- nucleophilic substitution reaction from protoporphyrin without purifying of the intermediate. The total yield of (3) is 90.6%. The effects of temperature, time and the dosage of reducing agent to (2) and the effect of pH and time to the yield of (3) were studied. The reasults show that the yield of (2) reaches a maximum of 98.3% in the molar ratio of hemin to Fe powder 1:1 and the the temperature of 120?C and the optimal reaction pH and reaction time are 10 and 6 h respectively with the yield of 92.1% in synthesis of product (3). The target products were characterized with ESI-MS, FT-IR and 1HNMR.