Abstract:This paper reported an optimum preparation process of 3-Picoline by mild liquid phase reaction of acrolein based on single factor design method. The reaction was carried out in the solvent of ethylene glycol monobutyl ether at temperature 140℃ for one hour, the mole ratio of acrolein and acetic ammonium and ethylene glycol monobutyl ether was 1:8:33, the mass ratio of acrolein and catalyst SO24-/TiO2-HZSM-5 was 1:1.4, and the mass percent of acrolein in n-butyric acid was 8%. Under the optimization conditions, the conversion rate of acrolein could reach to 100% and the selectivity of 3-picoline with a yield 49.92%

Abstract:Palm methyl ester was employed to synthesize palmitoyl ethanolamide and palmitoyl diethanolamide in the presence of KOH. The yield of palmitoyl ethanolamide and palmitoyl diethanolamide was 92.2 % and 89.0 %, respectively. The properties of palmitoyl diethanolamide and coconut diethanolamide were compared. The palmitoyl diethanolamide and coconut diethanolamide have similar surface tension and emulsifiability, while palmitoyl diethanolamide present weaker foaming ability than coconut diethanolamide did. The addition of decanoyldiethanolamide can improve foaming ability of palmitoyl diethanolamide; a mixture of decanoyldiethanolamide to palmitoyldiethanolamide (1:2.5, mol:mol) present similar foaming to that of coconut diethanolamide, which is twice as high as that of palmitoyl diethanolamide.

Abstract:The carboxymethyl starch was prepared by dry method using the cassava starch, mechanically activated for 60 min, as a starting material. The static adsorption behavior of the carboxymethyl starch , the adsorption thermodynamics and kinetics of the the carboxymethyl starch on Cu（Ⅱ）were investigated, meanwhile the product was characterized and the adsorption mechanism was stutied. The results show that the adsorption characteristic of carboxymethyl starcht on Cu（Ⅱ） is adapted to Freundlich and Langmuir adsorption isotherm equation. The adsorption thermodynamic parameters including enthalpy change △H, free energy △G change and entropy change △S were all negatived under the temperituer of 303K, 313K and 323K. The adsorption of the Cu（Ⅱ） on the carboxymethyl starch was an intraparticle diffusion process, and the adsorption mechanism including physical adsorption, ion-exchange and coordination.

Abstract:The objective compounds, benzyltriethylammonium tetrafluoroborate([Nbz222]BF4), benzyltriethylammonium hexafluorophosphate([Nbz222]PF6), benzyltriethyl-ammonium hydrogen sulphate([Nbz222]HSO4), benzyltriethylammonium dihydrogen phosphate ([Nbz222]H2PO4), and benzyltriethylammonium imidazolideintermediate([Nbz222]Im) were designed and synthesized by anion exchange reaction of the intermediate benzyltriethylammonium chloride which was prepared using triethylamine and benzyl chloride as starting materials. All the compounds including the quaternary ammonium-type ionic liquids(ILs) were characterized by FT-IR, 1H NMR, 13C NMR, ESI-MS and element analysis respectively. Meanwhile, the physical properties of the ILs were investigated. It was found that the melting points of the ILs are below 100℃ except for [Nbz222]PF6. The TG results indicated that the thermostability of [Nbz222]HSO4 is higher than the others associated with the decomposition temperature decrease in the orders of [Nbz222]HSO4 > [Nbz222]BF4 > [Nbz222]Im > [Nbz222]H2PO4. In addition, the ILs exhibited water absorption and were miscible well with polar solvent.

Abstract:To probe the rule of nitriles hydrolysis in high temperature liquid water with carbon dioxide, the effect of carbon dioxide pressure on phenylacetonitrile hydrolysis in high temperature liquid water was investigated, and the effects of carbon dioxide pressure and reaction temperature on pH of reaction system were calculated. The results show that the rate constants of hydrolysis at 0, 0.2 and 0.4 MPa carbon dioxide pressure were 6.2 × 10-4，4.1 × 10-4，3.0 × 10-4 min-1 at 473.15 K, respectively. And the corresponding pH values were 5.6、4.1、3.9. Since the base-catalytic mechanism is dominant in phenylacetonitrile hydrolysis, carbon dioxide can’t promote the hydrolysis of phenylacetonitrile efficiently.

Abstract:3,4-thiadiazol-2-one with 1,4-dibromobutane which was then demethylated then intramolecular alkylated. 5-Methoxy-3H-1, 3, 4-thiadiazol-2-one was synthesized by three steps with CS2, CH3OH and KOH as raw materials.The structures of the compounds were characterized by 1H NMR and 13CNMR spectra. The crystal structure of target compound was determined by X-ray single crystal diffraction. Target compound belongs to the triclinic, space group P1, with a =7.8400(16) ? b =10.464(2) ? c =10.514(2) ? α=63.84(3)? β=79.62(3)? γ=89.42(3)? V =759.2(3) ?, Z =4, wR(F2) =0.125, μ=0.37mm-1。

Abstract:Glutaraldehyde is prepared with cyclopentene as material,tungstic acid as catalyst,tert-butanol as solvent and hydrogen peroxide as oxidation in the microchannel reactor.The effects of the tungstic acid catalyst dosage,reaction temperature,residence time and additives on the experimental are evaluated.Optimal experimental conditions:the molar concentration of tungstic acid catalyst is 0.02mol/L,reaction temperature is 40℃,residence time is 4.5h;When adding KBr,the molar concentration of KBr is 0.02mol/L,residence time is reduced to 2h,conversion rate of cyclopentene is greater than 98%,selectivity is up to 93%.Studies have shown that application of microchannel reactor to improve the selectivity of this reaction is due to the unique structure of the reactor can control the intermediate generation and conversion process.For such a complex reaction of intermediate process,we can get the desired response effect by controlling the residence time to complete the puzzle for ordinary reactor.

Abstract:2-fluoro-5-bromonitrobenzene was prepared from 2-fluoronitrobenzene using the solvent acetic acid (CH3COOH) instead of sulfuric acid or 2-fluoro-5-bromonitrobenzene was prepared from 2-fluoronitrobenzene using the solvent acetic acid (CH3COOH) instead of sulfuric acid or boron trifluoride, using N-bromosuccinimide (NBS) as bromide reagent. The reaction condition was mild and easy to be controlled, the target product qualitative was analysised by GC-MS and quantification was analysised by GC. The best yield(98.6%) of 2-fluoro-5-bromonitrobenzene and conversion (100%) of 2-fluoronitrobenzene were obtained under optimized conditions that n(2-fluoronitrobenzene):n(NBS) =1:1.05, the reaction temperature was 10 ℃ and the reaction time was 2 h. The repeat experiments showed that the technology had a good repeatability under above optimum conditions.

Abstract:Abstracts:In order to evaluate the safety of starch-based alkyl polyglycosides, the acute dermal toxicity test of mice, acute eyes and skin stimulation tests on rabbits, multiple eyes and skin irritation and skin allergy tests on rabbits were conducted according to the standard GB7919-78. The results showed that the C0810、C1200、C1214 starch-based alkyl polyglycosides surfactant had no acute dermal toxicity and eye stimulation. They didn’t cause irritation or allergy to skin. The allergic reaction rate is 0. Thus they are more secure and reliable in practice.

Abstract:The styrene-maleic anhydride copolymer (SMA) was modified by alcohol. The effect of modified-conditions, such as reaction time and temperature, amounts of catalyst, amounts of alcohol on degree of esterification was further investigated. FTIR results showed that the anhydride in SMA successfully reacted with alcohols. The degree of esterification reached to 35% when molar ratio of isobutanol to SMA was about 12%, the mass ratio of p-toluenesulfonate was about 1%, and the reaction temperature was 80oC for 4 hours. The modified-SMA (SME) showed an excellent dispersing ability for carbon black. The ultrafine carbon black dispersion with 160nm would be obtained when degree of esterification was higher than 15%, the mass ratio of SME to carbon black was about 20%, and pH value was 9. The prepared carbon black dispersion with SME showed an improved stability to temperature and centrifugal forces.

Abstract:The oxidation of cyclohexane catalyzed by N-hydroxyphthalimide(NHPI) and cobalt sulphonated phthalocyanine(CoSPc) was investigated, in which GC was used to analyze the composition of oxidation products, except the normal products cyclohexanone and cyclohexanol, cyclohexanol acetate was fond and verified, according to standard sample. The effect of reaction time, temperature, the amount of NHPI and/or CoSPc were examined, the optimal reaction conditions of cyclohexane oxidation were as follows: reaction time 2 h, reaction temperature 80℃, n(Cyclohexane) : n(NHPI) = 10:1, n(NHPI) : n(CoSPc) = 6:1. Under the optimal conditions, the 10.5% yield of cyclohexanone, 1.1% of cyclohexanol and 0.4% of cyclohexanol acetate were gotten, and the total yield reached 12.0%.

Abstract:The improved procedure for preparing N-n-butylthiophosphoric triamide was described. The important intermediate N-n-butylaminothiophosphoryl dichloride was synthesized from thiophosphoryl chloride reacted with n-butylamine in the tubular reactor, followed by ammonolysis by NH3 for about 3h to give the title compound. The overall yield was 65.1%. The structure of the product was characterized by IR、ESI - MS、1H - NMR and 13C - NMR. In the meanwhile, a few factors including molar ratio of raw materials, reaction temperature and residence time are investigated. And the optimum condition were: Molar ratio of thiophosphoryl chloride to n-butylamine is 1 : 1.5, residence time is 30s, tube length 14m, tube diameter 3mm, 28 ~ 30℃。

Abstract:8-chlorodibenzo[b,f]thiepin-10(11H)-one, a key synthetic intermediate of Zotepine, was synthesis by metal-catalyzed coupling reaction, Willgerodt-Kindler rearrangement, hydrolysis and intermolecular cyclization reaction. The coupling reaction was catalyzed by CuI/L-proline, reaction temprature could be cooled down to 100 oC with a higher yield, 85%. Willgerodt-Kindler rearrangement and hydrolysis was carried out in a one-pot-reaction. The mole yield of all four steps is 40%. Product structure was identified by IR, Ms, and H 1NMR.

Abstract:In order to recover caprolactam from wastewater in the production of caprolactam from toluene, the behavior of caprolactam extraction with chloroform as extractant was studied. The influences of the pH of the solvent, extraction temperature and contact time on the extraction process were investigated. The experimental results showed that the extraction process is a fast extraction process. The distribution ratio increases with the increase of pH of the aqueous solution and reaches its maximum when pH=7. It was found that ammonium sulfate and 1-sulfonic acid-1-cyclohexanecarboxylic acid in the aqueous solution have the salting-out effect which can enhance the distribution ratio. The extraction temperature has only a little effect on the extraction process. The distribution equilibrium relation of caprolactam with chloroform in aqueous and organic solution with pH=7 was determined and the extraction enthalpy of 2.86 kJ?mol-1 was obtained by experimental measurement. When the volume ratio of organic to aqueous phase is 1, the recovery yield of 3-stage cross-flow extraction is above 98%. The results of cross-flow extraction for industrial wastewater with Chloroform showed that Chloroform is the suitable solvent for the recovery of caprolactam from industrial effluent.

Abstract:A Series of novel fluorine-containing Schiff-bases were obtained from 2-(4-amino-phenyl)-1,1,1,3,3,3-hexafluoro-propan- 2-ol and benzaldehydes via room temperature grinding by solvent-free reaction at room temperature without any catalyst. The products were identified by EA, 1H NMR, IR and MS spectra. Compared with conventional process, the yields of Schiff-bases were increased from 71%-87% to 98%-99%, but the reaction time were shortened from 90-240min to 10-50min by solvent-free reaction.

Abstract:Sarcinochrysis marina Geitler polysaccharide(SMP-0) was degraded by H2O2-Vc solution system. After separation and purification by Sepherose6B, three kinds of relative homogeneous products were obtained (SMP-1、SMP-2、SMP-3). The physicochemical properties of different polysaccharides were analyzed and the antioxidation, hygroscopicity and moisture retention activities were evaluated by determining the total reducing capacity, the scavenging ability of free radicals and moisture retention ratio. The results showed that SMP-0, SMP-1, SMP-2 and SMP-3 were sulfated polysaccharide and consisted of arabinose, D+fructose and glucose, but the molar ratio of each sugar had small difference. The antioxidant abilities were inverse proportion to molecular weight of polysaccharides, and showed dose-dependence. The total reducing ability of SMP-3 was closed to Vitamin C. The maximum scavenging activity of SMP-3 on O2-• and •OH were 94.89% and 88.98%, respectively. The hygroscopicity and moisture retention activity of high molecular weight (MW) polysaccharide was superior to that of low MW fragments. The maximum hygroscopic ratio of SMP-0 was 49.18%, which was 8.7% lower than that of glycerol, but was 27.4% and 35.2% higher than that of hyaluronic acid and chitosan, respectively. The maximum moisture retention ratio of SMP-0 was 77.23%, which was obviously higher than that of glycerol (30.02%), but was appreciably lower than that of hyaluronic acid and chitosan.

Abstract:In this paper, WPC-isomalto-oligosaccharide conjugate was prepared　by Maillard reaction. Response surface methodology was used to optimize Maillard reaction factors in order to get Maillard reaction products with the highest degree of graft. The results indicated that reaction temperature 90 ℃, weight ratio of WPC to IMO 1:3.125, pH 9.86 and reaction time 78.57 min were the optimum reaction conditions. On these conditions, the highest degree of graft was 25.75%. It was confirmed that the predicted and measured degree of graft values are consistent. At last the glycosylation of WPC was confirmed by SDS-PAGE.

Abstract:The antioxidant activities of two groups of Homalium paniculiflorum stem extracts, accelerated solvent extracts and conventional solvent extracts, were evaluated respectively with microplate reader, by DPPH method and FRAP method, taking ascorbic acid (Vc), butylated hydroxytoluene (BHT) and rutin (Rutin) as positive controls. Results showed that among these extracts, ASE-EtOAc extract had the strongest (yet weaker than all positive controls) capacity of DPPH free radical scavenging (EC50=20.8 μg/mLASE-DCM had the strongest (stronger than BHT yet weaker than Vc and Rutin) reduction capacity of Fe3+(FRAP value=793.3±45.7 mol TE /g);conventional water extract W displayed the weakest capacity in either DPPH free radical scavenging or Fe3+ reducing. Judging from comprehensive comparison, conventional NBA extract has better applied prospect and is worthy of extensive research, for it is easily prepared and has noticeable antioxidant ability.

Abstract:The flowers and leaves of Michelia champaca Linn. have got a strong nice scent. In order to find out their value for exploitation and utilization, the constituents of volatile oils extracted with SDE from the leaves, flowers and fruits of Michelia champaca Linn. collected in June were analyzed by techniques of GC-MS-computer. Seventeen, thirty-five and thirty-eight compounds were identified from the above three organs with SDE, respectively. The identified relative contents of the three kinds of essential oils are 92.18%, 99.23% and 98.93%, respectively. There are some differences among the chemical constituents of the three kinds of essential oils. The main constituents are beta-Linalool, germacrene B, caryophyllene, eucalyptol, β-elemene etc. The volatile oils from Michelia champaca Linn. are abundant in the high bioactive compounds with very important uses for perfume and medicine industry．

Abstract:Four compounds of 4-(3′-Chlorophenylamino)-6-methoxy quinazoline compounds, including 7-(3-(4-nitrophenoxy)propoxy)-N-(3′-chlorophenyl)-6-methoxyquinazolin-4-amine,7-(3-(3-nitrophenoxy)propoxy)-N-(3′-chlorophenyl)-6-methoxyquinazolin-4-amine,4-(3-(4-(3′-chlorophenylamino)-6-methoxyquinazolin-7-yloxy)propoxy)-3-methoxybenzaldehyde、3-(3-(4-(3′-chlorophenylamino)-6-methoxyquinazolin-7-yloxy)propoxy)-4-methoxyb- enzaldehyde, were synthesized from N′-(5-(3-chloropropoxy)-2-cyano-4-methoxyphenyl)-N, N-dimethylformamidine by cyclization，etheration, in the yield of 51.3%、60.3%、85.4% and 79.4% respectively. Their structures were characterized by IR, 1H NMR, 13C NMR, MS and elemental analysis. Preliminary bioassay indicated that some compounds possess antitumor activity to Bcap-37 cells in vitro by MTT method. The antiproliferation activity of compound Ιa to Bcap-37cells at the concentration of 10 μmol?L-1 was 83.4%.

Abstract:Double thiadiazole were synthesized by 5-amino-1,3,4-thiadiazoles, which was synthesized from thiosemicarbazide with 1,3-Dibromopropane. And a series of double thiadiazole-basedα-Aminophosphonates were accepted by a reaction of different aldehydes and phosphates. The structures of these compounds were confirmed by UV, IR, 1HNMR , 31PNMR and elementary analysis. Preliminary bioassay showed that they all have excellent fungicidal activities against Botrytis cinerea, Gibberella zeae, Physalospora pinicola and Rhizoctonia solani .

Abstract:The purpose of the study was looking for the novel compounds with herbicidal activities. Intermediate 4-(4,6-dimethoxypyrimidin-2-yloxy)-2-methylbenzaldehyde(3) was synthesized using m-cresol as starting material by acylation reaction and substitution reaction. Twelve novel 2-(4-(4,6-dimethoxypyrimidin-2-yloxy)-2-methylphenyl)-2-(substituted phenylamino) acetonitrile derivative compounds have been synthesized using intermediate (3) via three component one-pot reaction, and the yields are 64～96%. The structures of all synthesized compounds were confirmed by 1H NMR, MS and elemental analysis techniques.

Abstract:NaA of microporous zeolites was prepared by hydrothermal synthesis method with molar ratio of n(SiO2)∶n(Na2O)∶n(Al2O3)∶n(H2O)= 1:1.5:0.5:100 at 90 ℃ for 3 h, then followed by the addition of chemicals to the microporous zeolite NaA with molar ratio of n(SiO2)∶n(NaOH)∶n(CTAB)∶n(H2O)=1:0.3:0.3:90, composite micro-mesoporous molecular sieve of NaA / MCM-41 was successfully synthesized at 110 ℃ for 24 h. The structures of composite materials compared with the mechanical mixture were characterized by powder XRD, SEM (EDS) and TEM. The results showed that: in 50 mL 20 mg/L cationic red X-5GN solution ,NaA / MCM-41 micro-mesoporous molecular sieve composite dosage is 1 g/L, pH is 6, the oscillation time is 60 min, the decolorization rate is 96.4 %, this adsorption decolorization effect is better than that of NaA zeolite and MCM-41 mesoporous molecular sieve. It can be used for further expanded test.

Abstract:Collagen fiber immobilized Zr(Ⅳ)(ZrCF) was applied in the treatment of high concentration arsenate and fluoride co-existing containing wastewater. Adsorption behavior of As(Ⅴ) and F by ZrCF in co-existing containing wastewater was investigated. Taking the high concentration arsenate and fluoride co-existing containing wastewater from fertilizer plant as example, the effects of adsorbent dose, initial pH and contact time on adsorption performance were studied and the column experiment was carried out. Results suggested ZrCF had stronger appetency to As(Ⅴ) than to F. When the adsorbent dose was above 0.8 g, the concentration of arsenate and fluoride in effluent satisfied the national discharge standard. pH6.0 was the optimal acidity value, and As(Ⅴ) and F content decreased to the limited value after 6 h. When the effluent volume was 4.68 L, the fixed bed was saturated to As(Ⅴ) and F , and ZrCF could remove arsenate and fluoride simultaneously and efficiently.

Abstract:4-(sec-butyl)-2,6-di-tert-butylphenol was synthesized from 4-(sec-butyl) phenol and isobutene using sulfuric resin as catalyst. The influence of the catalyst, reaction temperature, reaction time, material ratio and catalyst dosage on the yield of the product had been investigated. The optimal reaction condition was using sulfuric resin as catalyst, choosing the amount of catalyst for 3%~5% (quality ratio), the molar ratio was n(4-(sec-butyl) butylphenol):n(isobutene)=1:2, the reaction temperature 90~100℃, the reaction pressure 0.15 ~0.2Mpa, the reaction time 4 hours. Under the optimal reaction condition, the conversion was more than 90% and selectivity was more than 95%. More than 97.5% of the 4-(sec-butyl)-2,6-di-tert-butylphenol was obtained by distillation separation.