Abstract:The Knoevenagel condensation reaction has been widely used to prepare fragrance, chemical materials and pharmaceuticals. With ionic liquids as reaction solvents, reactions of a wide range of aldehydes and ketones with methylene compounds proceed smoothly. Functional ionic liquids as catalysts can successfully catalyze Knoevenagel reactions in the absence of any other catalyst. Ionic liquids, as “green” and “designer” solvents, provide a high efficient and environmental friendly approach for Knoevenagel reactions. In this paper, the progress in the use of ionic liquids for Knoevenagel condensation reaction is reviewed.

Abstract:In order to enhance the aging resistance and permeability of acrylate used as protection of damaged seriously silicate cultural relics, nano SiO2 obtained by acid-catalyzed hydrolysis reactions of tetraethoxysilanewas added to polyacrylate via blending method. The physical appearance，viscosity，glass transition temperature，molecular structure and physical properties of composites were evaluated by spectrophotometer，advanced rotational rheometer，DSC, ATR-FTIR and SEM. The selected modified material was used for protection of pottery samples，the permeability and compressive strength of the treated samples were tested. The results indicated the modified material A7 added 7.0 percent of silica sol gave transparent membranes, obtained better thermal resistance, aging resistance and penetration. What’s more，A7 had excellent performance in the protection of the damaged seriously silicate cultural relics.

Abstract:Polybenzidine was synthesized by interfacial polymerization under various monomer oxidant molar ratio. Effects of monomer oxidant molar ratio on morphology, structure, and properties of polybenzidine were studied by techniques of Fourier Transform Infrared Spectroscopy (FT-IR), Ultraviolet Visible Absorption Spectroscopy (UV-vis), Transmission Electron Microscopy (TEM), X-ray Diffraction (XRD), and Cyclic Voltammetry (CV). The results showed that all of the samples were microrod-like and the surface of the microrods was smooth and uniform. The changes of monomer oxidant molar ratio had no obvious effect on the morphology of the polybenzidine. The results of structural analysis and cyclic voltammetry indicated that the monomer oxidant molar ratio should not be very high or very low to obtain the polybenzidine with the optimal degree of conjugation, order arrangement of molecular chain, and the best electrochemical behaviors. The suitable proportion in this work was 1:1.

Abstract:This article presents efficient syntheses of two labeled standards [13C6]leucocrystal violet and [13C6]violet crystal with 13CH3OH as the common substrate. Esterification of p-toluenesulfonyl chloride with 13CH3OH provided [13C]methyl p-toluenesulfonate, which was used to methylate aniline to give [13C2]N,N-dimethylaniline. Condensation of [13C2]N,N-dimethylaniline afforded [13C6]leucocrystal violet and [13C6]violet crystal. Both products were shown by NMR and LC-MS to be target compounds. Their chemical purities are higher than 99 % and isotopic enrichment are higher than 98.5 %.

Abstract:Synthesis a nitrogen-containing 15-membered triolefinic macrocycles by five-steps method[(E,E,E)-1,6–Bis[(2,4,6-triiso-propylphenyl)sufonyl]-11-[(4-fluorophenyl)sulfonyl]-1,6,11-triazacyclopentadeca-3,8,13-triene] with 1,4-dibromo-2-buten, 4-fluorobenzenesulfonam, 2,4,6-triisopropylbenzenesulfonamide as the main reactant. The surface group of the 2.0 generation poly(propyleneimine) dendrimer(2.0G PPI) , which is prepared by the co-worker of the laboratory, is modified by the 15-membered triolefinic macrocyclic compounds to synthesis hybrid poly(propyleneimine) dendrimer. The products were proved to be in accord with the theoretical structure by characterization with infrared and nuclear magnetic resonance spectroscopy.

Abstract:In this paper, AR（Aromatic Resin）pitch as raw materials, high performance activated carbons were prepared by chemical activation method. The specific area and porosity of the activated carbon samples were studied by the nitrogen adsorption. Furthermore, the simulative supercapacitors were assembled with the resultant carbons, and their electrochemical performances were investigated by charge-discharge of constant current, Cyclic voltammetry. The results showed that the discharge efficiency of simulative supercapacitors kept above 90% after 300 cycle tests, and the average specific capacitance reached 187.8 F•g-1 at 50 mA•g-1 current density and 131.5 F•g-1 at 500 mA•g-1 current density. The specific capacitance retention was 71.3%, the capacitance attenuation ratio was 4.0%.

Abstract:Ethylene glycol gemini sodium 2-methyl-1-pentyl sulfosuccinate was synthesized through an environmentally-friendly process, which was under normal pressure and in the order of single-esterification, sulfonation and diesterification, using carbonyl solid acid as the catalysis of esterification, without purification and separation to the intermediates. The optimum conditions were studied and concluded as follow, in the single-esterificatino, n(maletic anhydride):n(2-Methyl-1-pentanol)=1.05:1.00, using alkyl sulfonate which was 1% of the amount of maletic anhydride as the catalysis, at 80℃ for 1h, the yield can be 98.88%. For the sulfonation, n(maletic anhydride):n(sodium hydrogen sulfite)=1.00:1.05, at 70℃ for 2.0h, the yield can be 98.71%. In the diesterification, n(maletic anhydride):n(ethylene glycol)=1.00:2.20, w(carbonyl solid acid)=3%, at 180℃ for 3.5h, the yield can be 95.05%. The surface tension and critical micelle concentration of the product were tested as 30.3mN/mol and 1.26?0-4mol/L.

Abstract:The effecting factors of degumming and deacidification for crude Jatropha oil were investigated with the activated clay loaded by the citric acid and the calcium hydroxide respectively. And then degumming and deacidification process were coupled together to strengthen refine process by one-step. The results indicated that the acid value is 0.23 mg KOH/g and the phosphatide content is 0.09 mg/g for refined Jatropha oil. When the refined oil was the feedstock using a homogeneous alkaline catalyst for biodiesel production, the content of methyl ester in the product is larger than 99%. The performance on biodiesel production has been satisfactory.

Abstract:SAPO-34/kaolin microspheres catalysts (SCKMs) were in-situ hydrothermally synthesized onto the NaOH-pretreated calcined kaolin microspheres (CKMs). The effect of the NaOH concentration within 2%~10% on the physicochemical properties of CKMs and the ensuing synthesized SCKMs were characterized by means of XRD, XPS, SEM, low-temperature N2 adsorption. The results showed that, NaOH solution had obvious effects on the chemical composition and the morphologies of the CKMs, and then the properties of the in-situ synthesized SAPO-34 catalysts. In comparison, the optimal NaOH concentration was 4%. For the MTO reaction catalyzed by the prepared 4-SCKM catalyst, 100% methanol conversion, 89.8% light olefins selectivity, 964 min lifetime have been obtained, which are better than that of the SAPO-34 catalysts not synthesized by in-situ method.

Abstract:2,10-Epoxypinane was synthesized by the epoxidation of β-pinene using acetonitrile-water as solvent, ketone as catalyst, hydrogen peroxide as oxidant. The effect of ketone, solvent, mole ratio of hydrogen peroxide to β-pinene , pH, reaction temperature and time on the yield of 2,10-epoxypinane was investigated. The results show that the yield of 2,10-epoxypinane could reach 79.6% and its content was 94.6% under the following reaction conditions: the proper catalyst was acetone, the mole ratio of hydrogen peroxide to β-pinene was 5:1, pH was 10.0 , reaction temperature was 30℃,and the reaction time was 8h. The product was characterized by data of GC, GC-MS spectrum, infrared spectrum and 1H NMR spectrum.

Abstract:The essential oil was extracted from Trollius chinensis Bunge by steam distillation extraction, simultaneous distillation extraction, ultrasonic extraction, homogenate extraction simultaneous distillation extraction followed ultrasonic extraction, simultaneous distillation extraction followed homogenate extraction methods. The constituents of essential oil were isolated and identified by GC-MS, and the applications of the oil in unblended cigarette flavoring were studied as well. The results showed that: 1) The extraction rate of oil extracted by the six methods was 0.20%, 0.67%, 2.31%, 2.67%, 0.82%, 0.78% and 20, 30, 19, 18, 37, 30 compounds were identified, respectively; the primary chemical components were β-ionone and dihydroactinidiolide, etc; among of them, the total amount of essential extracted by ultrasonic extraction, homogenate extraction are higher relatively, but they more impurity, the oil extracted by simultaneous distillation extraction followed ultrasonic extraction is better than the others. 2) It could play an important role in enhancing the aroma quality of cigarette, obviously reducing the irritation, and smoothing the smoke while essential oil of simultaneous distillation extraction followed ultrasonic extraction is better than the others.

Abstract:The volatile components of Plum were identified by method of HS-SPME—GC-MS. There were 66 volatile compounds, including 8 alcohols, 4 lactones, 12 aldehydes, 23 esters, 2 ketones, 8 acids, 7 terpenes and terpene alcohols and 2 aromatic compounds. The reasons why plum showing peach, milk and apricot fruit aroma in the early, middle and late stage of aroma production were analysed.

Abstract:An efficient procedure for the alkylation, diazotization and oxyalkylation of 2-amino-6-chloropurine to 2-Chloro-6-methoxy-9-alkylpurine compounds in good to excellent yield is reported. The synthesized compounds were characterized by MS, 1H NMR and elemental analysis. The effects of solvent, mole ratio of raw material, catalyst and reaction temperature on the alkylation reaction were discussed, and the yields of the compounds of this step were more than 76% under optimized conditions that n (2-amino-6-chloropurine): n (bromoalkane) = 1:3, n (bromoalkane): n (K2CO3) = 1:1.5, reaction temperature was 20℃ with DMF as solvent.

Abstract:Trimethylolpropane maleates(TMPMs) are prepared by esterification from trimethylolpropane(TMP) and maleic anhydride(MA). The effects of feed ratio, temperature, reaction time and catalyst are studied, the results indicated: esterification rate of MA can reach 100% with n(TMP)/(MA)=1:2 under 90℃ during 120min, esterification rate of MA can reach 100% with n(TMP)/(MA)=1:2.5 under 90℃ during 240min, for n(TMP)/(MA)=1:3, esterification rate of MA reach 90.7% under 90℃ during 240min and will not change any more. Catalyst addition is helpful for increase of esterification rate of MA, which can reach over 99% without diesterification of MA. The structure and composition of TMPMs are characterized and analysed by NNM R, the Average Double Bond Functionality(ADF) of TMPMs are calculated by esterification rate.

Abstract:Retanning fatliquor agent amphiphilic copolymer(PNMA)was synthesized from hydrophobic monomers N-octadecyl maleic amide(NSA-18) and octadecyl methacrylate(MAO), hydrophilic monomer acrylic acid (AA), with ammonium persulfate(APS) as initiator by free radical water emulsion copolymerization during which active monomer was added dropwise.The structure of PNMA was characterized by means of FT-IR and DSC. Effect of reaction conditions on properties of PNMA were investigated by single factor experiments. under optimal conditions: mole ratio of NSA-18 to MAO3:2, mole ratio of hydrophobic monomer to hydrophilic monomers 1:3.5, mass fraction of ammonium persulfate 4.5%(base on total mass of monomer), reaction temperature 88℃, dropping time of active monomer 2h, the retanning fatliquor agent showed good thickening rate,softness and `waterproofness. Light transmittance of 1% (mass fraction) PNMA aqueous emulsion obtained was 42.7%, the thickening rate was 29.6%, and static water absorption was appropriately 43.6%.

Abstract:Novel water-soluble macromolecular UV absorber PVAm-g-BP-4 was synthesized with 2-hydroxybenzophenone as UV absorbing group and polyvinylamine (PVAm) as backbone. PVAm-g-BP-4 was synthesized through 2 steps. Reactive intermediate 2-hydroxy-4-methoxy-5-chlorosulfonylbenzophenone (CBP-4) was first synthesized from 2-hydroxy-4-methoxy-5-sulfo-benzophenone (BP-4) with thionyl chloride as chlorination agent and solvent and N, N-dimethylformamide (DMF) as catalyst, the yield of the intermediate could reach 94.5%. And then PVAm-g-BP-4 was synthesized by grafting CBP-4 onto PVAm. CBP-4 was confirmed to be grafted onto PVAm through TLC, IR and UV spectroscopy. The preparation conditions of the intermediate and product were optimized by studying the dosage of catalyst, reaction temperature, reaction time, solvents ratio, etc. Application of PVAm-BP-4 on cotton fibers shows it provides the fibers good anti-UV property and its wash fastness was satisfactory.

Abstract:Medium-molecular weight sodium polyacrylate for ceramic superplasticizer was synthesized from acrylic acid as monomer, while ammonium persulfate/sodium bisulfite as redox initiator, sodium bisulfite as reducing agent. We investigated the factors having effects on the polymer’s average molecular weight such as redox system, monomer, and temperature. Moreover, the fluidity and dispersing properties in the ceramic slurry were investigated after adding polymers. The optimum reaction conditions for synthesizing ceramic superplasticizers are as follows: the adding amount of ammonium persulfate is 0.8 %, the amount of sodium bisulfite is 10 %～12 %, the mass fraction of acrylic acid is 24 %～26 %, reaction temperature is 70℃～80℃. The synthesized superplasticizer was characterized and analyzed by FT-IR and GPC, and the effects of different reaction conditions on the viscosity and dispersion of ceramic’s slurry were investigated. The results show that the slurry’s negative Zeta potential increases from 27.4 mV to 78.4 mV when the concentration of polymer is 1000 mg/L. And the minimum value of slurry’s viscosity is 179 mPa•s when the concentration of sodium polyacrylate is 0.25% (based on the absolute dry slurry). The ceramic body with composite components of polymer and sodium tripolyphosphate (w/w=1:1) has higher bending strength, which is increased by 33.33%.

Abstract:The effect of the acetylenic-modified polysiloxane emulsion defoaming agent on the surface tension, density, viscosity, pH value and writing performance of the gel ink was investigated. The results showed that the surface tension of the gel ink decreased slightly and the viscosity and pH value of the gel ink were not affected by adding the defoaming agent. The optimizational dosage of defoaming agent was 0.042wt%~0.043wt%. The pens filled with such gel ink behave good writing performance. And the uniformity of the amount of the gel ink consumed during writing was improved.

Abstract:Modified polycarboxylate superplasticizer (MPC) was synthesized by free radical copolymerization of acrylic acid (AA), methyl acrylic acid sodium (MAS), β-cyclodextrin grafted maleic anhydride (MAH-β-CD) and methylacrylic acid polyethylene oxide ether (APEG) using ammonium persulfate [(NH4)2SO4, APS] as initiator. Effects of mole ratio of reactants, dosage of initiator, reaction temperature and reaction time on the properties of superplasticizers were investigated. The optimum MPC was synthesized when the molar ratio of n(AA) : n(MAS) : n(MAH-β-CD) : n(APEG) were 5 : 0.5 : 0.1 : 1 using 5 wt% APS at 90 °C for 5 h. The application results show that the fluidity of cement paste can reach 306 mm, the initial setting time is 440 min and the water reducing ratio is 32.2 %. SEM and compressive strength results show that the microstructure of hardened cement doped with MPC are more homogeneity and the porosities are smaller, which are benefit for the development of later structure of concrete.

Abstract:The ammonium persulfate is used to oxidize the alkali lignin to prepare oxidized alkali lignin with low molecular weight and more polar functional groups. The prepared high-performance lignin-based grinding aid GCL6-J is evaluated by grinding experiment, the results show that the 45μm screen residue values of the milled cements decrease from 7.8% to 5.3% at the dosage of 0.1% (occupy the total clinker and composite materials by mass), which is equivalent to the 89.3% grinding effect of triethanolamine. The long-term breaking and compression strengths of the milled cement using GCL6-J reach or exceed those of triethanolamine. The combination property evaluation indicates that the GCL6-J belongs to lignin-based high-performance grinding aid. The XPS spectrum analysis shows that the thickness of the adsorption layer of the oxidized alkali lignin is 1.02nm (calculated by the Si), while that of the alkali lignin is 0.41nm. The C1S content of the milled cement using GCL6-J decreases from 38.11% (blank) to 34.07%, while the Ca2p and Si2p contents increase from 8.51% and 4.42% (blank) to 10.29% and 4.98%,respectively, which demonstrates the grinding mechanism of GCL6-J in the milling process: adsorbs on the new-born high energy active sites of the cement surface and masks the charge.

Abstract:Six 2-aryl-substituted imidazoles were prepared from corresponding nitriles, which was reacted with aminoacetaldehyde dimethyl acetal through three steps by one-pot method. From study on the effects of sodium methoxide amount, temperature and time of cyclization reaction, the optimum conditions were investigated that the mole ratio of the amount of sodium methoixde to the starting nitriles was ( 0.08～0.12): 1, the cyclization reaction temperature was 80～90℃ and the cyclization reaction time was 3～8 h. The structures of all products were characterized by melting point, Mass, 1HNMR and elemental analysis.

Abstract:1,2-Disubstitued benzimidazoles were selective synthesized in excellent yields by the condensation of o-phenylenediamine with aromatic aldehydes under mechanically activated solvent-free conditions in ball mill using FeCl3•6H2O as the catalyst. Structures of products were characterized by 1H NMR, 13C NMR and HRMS. The optimum conditions were given: n (FeCl3•6H2O) : n (o-phenylenediamine) : n (aldehydes) = 0.25 : 1 : 2 and the ball mill was run with a rotational speed of 400 r/min for 2 h. The reaction was carried out without solvent and just needed a simple work-up procedure. This mild and eco-friendly method had the potential for facile preparation of benzimidazole derivatives.

Abstract:In this study, cationic etherifying agent 2,4-bis(dimethylamino)-6-chloro-[1,3,5]-triazine (BDAT) was synthesized by ultrasonic-assisted with cyanuric chloride and dimethylamine as raw materials. It was found that heterogeneous solid–liquid reaction can be proceed by ultrasonic-assisted in aqueous solution. Effects of reaction conditions including ultrasonic time, temperature, pH, ratio of the reactants and ultrasonic irradiation power on the yield of BDAT were studied. The yield of the target product reached 96% under the optimum conditions. The structure of the product was confirmed by IR, 1HNMR and MS spectroscopy.

Abstract:Polyether-grafted Polysiloxanes was synthesized by microwave irradiation from methyl hydrogen silicone Polyoxyethylene polyoxypropylene acetate, The optimum reaction conditions were determined as follows: radiation power of 600w, the molar ratio of polyether and silicone of 1.2:1, amount of chloroplatinic acid catalyst 10mg/kg, temperature of 90℃ and 40min microwave irradiation. Under the optimum conditions, the everage conversion ratio was 94.7%. The structure of sample was analyzed and characterized by method of FTIR and 1H-NMR. Polyether-grafted Polysiloxanes was used to produce antifoaming agent and applied in metal cleanser. The results showed that the antifoaming agent demonstrate superior antifoaming performance and washing effect, better stability．