Wang Yingying , Wang Bin , Huang Yuewen , Xie Haining
2018, 35(2).
Abstract:We prepared the polystyrene/graphene oxide core-shell microspheres (PS/GO) based on the self-assembly between graphene oxide sheet (GO) and cationic polystyrene microspheres (PS) through electrostatic and π-π attraction between them and the PS/GO were reduced by hydroiodic acid (HI) to obtain the polystyrene/reduced graphene oxide core-shell microspheres (PS/rGO), which were characterized byXRD, SEM and TEM. It was found that the thickness of shell GO was influenced by ultrasonic and mechanical stirring, self-assembly time and GO concentration. The PS/rGO composites with different amount of shell rGO were characterized by conductivity and thermal stability measurements and the results show that the shell rGO will directly affect its conductivity and thermal properties. Besides, the conductivity and thermal stability of PS/rGO were improved compared to PS due to the special core-shell structure: the electronic resistance of PS (17.3 Ω) were down to 8.34 Ω (PS/rGO) and the initial thermal decomposition temperature of PS/rGO were increased by nearly 120 ℃.
2018, 35(2):0-0.
Abstract:humic acid/acrylic acid-urea controlled release superabsorbent resin with interpenetrating polymer networks was prepared by solution polymerization using acrylic acid(AA) urea and humic acid(HA) as raw materials, N`N-methylenebisacryla mide as crosslinkingagent and ammonium persulfate as initiator, respectively. The effect of the neutralization degree acrylic acid, reactant ratio, reaction temperature, the amount of initiator and cross-linking agent on the water absorbent ability were investigated. In addition, The structures and performance of products were studied by FTIR、SEM、DSC and Pressure potential method.The results show that the obtained superabsorbent resin has maximum waterabsorption ability up 310g/g, available water rate up to 93.81% and has good water retention performance when the polymerization temperature is 80℃, the amount of initiator,crossing agent, humic acid and urea in the acrylic acid were 0.3%, 0.06%, 20% and 50% respectively.
2018, 35(2):0-0.
Abstract:In this paper, graphene oxide (GO) was firstly modified by aminosilane coupling agent, and nano silver was loaded by adsorption and reduction. Then, organic-inorganic hybrid microfiltration membrane was prepared with modified GO and hydrophilic polymer such as polyvinyl alcohol (PVA) through the nonsolvent induce phase separation (NIPS) method. The structure of the prepared Ag@mGO and the hybrid membranes were characterized and identified by FTIR, XRD, TEM, SEM, Contact Angle (CA), Porosity (ε) and MeanPore Size (rm).The antibacterial property, filtration performance and antifouling ability of the hybrid membranes were characterized meanwhile bycorresponding measurements.The results show that the Ag@mGO particle size is below 10 nm and the silver loading is 5.45%. The porosity (ε) is 30% ~ 40% and the average pore size (rm) is 0.54 ~ 0.71 μm, which means good hydrophilicity and excellent filtration performance. At the same time, the rejection rate (R) for BSA was above 80.2%, and the diameter of the inhibition zone for E. coli (K12) was above 1.29 cm, which indicated that the prepared hybrid microfiltration membranes also had good resistance to BSA pollution and antibacterial efficacy.
2018, 35(2).
Abstract:3- butyl -5,5-dimethylhydantoin Ammonium Salt (BDMH)was Synthesized. The product was separated and purified by column chromatography and thin layer chromatography. The structure of BDMHI were characterized by Fourier transform infrared spectroscopy (FTIR), H- nuclear magnetic resonance spectrum (1HNMR), C- nuclear magnetic resonances spectrum (13CNMR). The corrosion inhibition performance and adsorption behavior of BDMHI for Q235 steel in 6% HCl solution were investigated using weight loss measurements, polarization cure , electrochemical impedance spectroscopy(EIS) methods and AFM. The results showed that BDMHI had excellent corrosion inhibition performance, and both cathodic and anodic processes of Q235 steel corrosion were suppressed. Inhibition efficiency increased with the increase of concentration, and The highest inhibition efficiency was 91.25%. We found that the adsorption of BDMHI on Q235 steel could be fitted to a Langmuir isotherm equation, and it belonged to a mix-type adsorption, which was mainly dominated by chemisorption.
2018, 35(2).
Abstract:The hypolipidemic and antioxidant effects of the polysaccharides from S. dimorphus residues were studied. The results showed that the polysaccharides from S. dimorphus residues have an inhibition for gaining weight, liver index and spleen index. They also could obviously drop the content of serum lipids TG and MDA, and enhanced the activity of SOD in hyperlipidemia rats. However, there is not obvious impact of the polysaccharides from S. dimorphus residues on the serum TC, HDL-C and LDL-C in hyperlipidemia rats. Therefore, the polysaccharides from S. dimorphus residues have significantly hypolipidemic and antioxidant effects. The results are useful for the high value utilization of S. dimorphus residues.
WANG Qing , WANG Li-qun , Qi Li-ying , Zhang Sen , ZHANG Jian-da
2018, 35(2):0-0.
Abstract:A strain of Yeast G5 was isolated from vineyard soil samples, which can catalyze asymmetric reduction of ethyl-2-oxo-4-phenylbutanoate (OPBE) to ethyl (R)-2-hydroxy-4-phenylbutyrate [(R)-HPBE]. It was identified as Rhodotorula mucilaginosa by its morphological and 18S rDNA sequence analysis. Various parameters affecting on asymmetric biocatalytic reduction of Rhodotorula mucilaginosa CCZU-G5 were investigated, and the optimal conditions were achieved, i.e. 35 ℃, pH 7.0, cell concentration 0.2 g/mL, 3.0% glucose (w/v), 3 mmol/L Ca2 . After reacting 12 h under the optimum conditions, the product yield would be up to 82% with 99.9% e.e. value.
mashasha , zhaozhenyu , liupinghuai , wangmeng , wuqiong
2018, 35(2).
Abstract:The non-volatile components of clove were extracted by microwave-assisted extraction (MAE), ultrasonic-assisted extraction (UAE) and Soxhlet extraction (SE). The optimal extraction method was chosen by the comparison of the content of total flavonoids and phenols and antioxidant activities. Meanwhile, the microstructure of clove powder was observed by scanning electron microscope (SEM). On the basis of single factor experiment, response surface methodology was designed to optimize the extraction process. The results showed that: the microwave-assisted extraction is the best method. The optimized conditions of MAE are 248 W, 52℃, 72% ethanol, 23.5min. Under the above conditions, the content of total flavonoids and phenols are 30.96% ± 0.44% (309.62 ± 4.41 mg/g) and 70.13% ± 0.86% (701.34 ± 8.64 mg/g), respectively. The results were consistent with the predictive values. The DPPH-scavenging activity was 99.78% ± 0.73%, the ABTS-scavenging activity was 99.07% ± 0.84%, the ferric reducing antioxidant power was 3.61 ± 0.21 mmol/L, the Fe2+ chelating capacity was 32.92% ± 1.12% and the anti-lipid peroxidation activity was 82.67% ± 2.46%. The non-volatile components of clove had excellent antioxidant activities.
JIA Jin , CHENG Lu , ZHANG Cheng , CAI Wei-jie , ZHOU Da-yong , GAO Xin-qin , LIU Zhongyuan , ZHANG Jiang-Hua
2018, 35(2).
Abstract:A kind of mesoporous niobium phosphate (m-NbP) solid acid catalyst was successfully synthesized via convenient hydrothermal method. The obtained catalyst was characterized by X-ray diffraction (XRD), Nitrogen adsorption-desorption, Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Temperature-programmed desorption of ammonia (NH3-TPD) and Infrared spectra of pyridine adsorption (Py-FTIR) etc in order to elucidate its structural and acidic properties. The one-pot conversion of glucose to 5-hydroxymethylfurural (5-HMF) in a biphasic water/DMSO medium was also investigated over the m-NbP catalyst. The catalyst dosage, volume ratio of water to DMSO, reaction temperature, reaction time, catalyst recyclability, comparison of catalytic performance with other three catalysts (Amberlyst-15, Nb2O5 and m-NbP-F127) etc were studied in detail. The results indicated that the catalyst exhibited the promising catalytic performance for 5-HMF production probably assigned to the porous structure and the adequate strong acid sites. The 5-HMF yield could be obtained as high as 47.0% at 170 ℃ within 1.5 h when the mass ratio of glucose to m-NbP and volume ratio of water to DMSO was 2:1 and 5:5 respectively. Noticeably, the m-NbP catalyst could be recycled up to 6 times without any obvious deactivation after high-temperature calcination-regeneration. This work was the continue efforts for the development of efficient solid catalyst for excellent conversion of one-pot glucose to 5-HMF.
LAO Wen-ting , ZHENG Lan , WANG Yu-qi , HAN Xiao-long , FAN Zhao-yun , ZHANG Qiao-ying , CHEN Kai-xun , SHAO Ji-sheng
2018, 35(2).
Abstract:The capsicum resin was used as raw material during the adsorption experiments, and the optimal technology and mechanism of capsaicin adsorption on the 201×7 anion exchange resin was determined by the method of static adsorption. The concentration of capsaicin was detected by visible spectrophotometry, and the adsorption isotherms at the different pH were obtained. The kinetics model of capsaicin adsorption by ion exchange was also established. Experimental results indicated that the optimal pH of capsaicin adsorption was 5.5, and the Langmuir equation was more suitable for the adsorption process when the pH was lower than 5.0 or higher than 6.0; the adsorption isotherms of capsaicin were in highly accordance with Freundlich equation when the pH ranged between 5.0 and 6.0. Under the optimal pH=5.5 and 308.15K, larger mass concentration of the capsicum resin would increase ion exchange speed significantly, and the stirring speed within 800r/min ~ 1200r/min can favor the adsorption process at the initial stage (<30min). By calculation, the adsorption rate constant, activation energy and reaction order were 2.11×10-3s-1, 12.6 kJ/mol and 0.268, respectively, and the kinetics equation of capsaicin adsorption on anion exchange resin was achieved under the optimal pH=5.5 through the solution of Freundlich model.
WANG Hong-qin , WANG Ya-ming , JIANG Li-hong
2018, 35(2).
Abstract:Supported [Rh(COD)Cl]2 catalysts were prepared. The resulting catalysts were characterized by means of XPS, N2 adsorption-desorption and FTIR analysis methods. The hydrogenation reaction of beta-pinene was used as probe reactions to investigate the catalytic performance. The effects of carrier type, oxidant燞NO3 concentration and Rh-loading on catalytic properties were optimized in details. On this basis, the hydrogenation conditions were investigated by orthogonal爀xperiment, and the catalytic use of [Rh(COD)Cl]2/AC was measured as well. The experimental results indicated that the catalytic activity of [Rh(COD)Cl]2 catalysts supported on activated carbon was greatly improved. The catalyst showed optimal catalytic activities with 99.0% conversion of beta-pinene, 89.0% selectivity of cis-pinane and 88.9% yield of cis-pinane when the optimal conditions for catalyst preparation were carrier type of activated carbon, HNO3 concentration of 35% and Rh-loading of 5%. The [Rh(COD)Cl]2/AC remained high activities with 89.64% conversion of beta-pinene after being used for four times. The cause of deactivation of [Rh(COD)Cl]2/AC was that active component Rh was easy to lose in the running process.
2018, 35(2):0-0.
Abstract:Benzotriazole and its derivatives are widely used as UV absorbers, due to their low toxicity and excellent stability. The catalytic performance of PdPtCu/C for the synthesis of 2- (2'-hydroxy-5'-methylphenyl) benzotriazole (UV-P) from 2-nitro- (2'-hydroxy-5'-methylphenyl) azobenzene (HAB) was studied. The conversion of HAB reached 100% and the selectivity of UV-P kept 92.2% after 5 h’ reaction at 323 K and 0.5 MPa hydrogen pressure. XRD, TEM and XPS results showed that the formation of Cu-Pd, Cu-Pt alloy phase and the proper amount of the noble metal species (Mδ ) on the surface of the catalyst were the key factors to inhibit the breakage of N-N bond and to reduce the by-reaction of excessive hydrogenation, which thereby supressed the formation of tetrahydrofins and aromatic amines by-products.
2018, 35(2):0-0.
Abstract:g-C3N4/ZnO heterojunction composites were in situ prepared through the one-pot approach. The photocatalytic activities of the samples were evaluated by the photodegradation of methylene blue (MB) under visible light irradiation and the mechanism of g-C3N4/ZnO photocatalytic reaction was investigated. XRD, FT-IR, SEM and UV-Vis DRS were used to characterize the obtained composites. The results show that the heterojunctions are formed by the tight coupling between g-C3N4 and ZnO, which improves the separation efficiency of electron-hole pairs and have stronger light response in visible region. With the optimal g-C3N4 mass fraction of 19%, the catalytic reaction kinetic constants of MB solution degradation was 0.0206min-1, which was 3.8 times that of pure g-C3N4. The regenerated catalyst still kept good catalystic performance after recycling 5 times.
chenjin , daibencai , huocuimeng , liuxiaoli , guoshengqiang , zhaoyongde
2018, 35(2).
Abstract:Ten novel salicylaldehyde-ɑ-aminophosphonate derivatives were synthesized through the condensation reaction (microwaved-assisted method) and NaBH4 as the reduction agent, using ɑ-aminophosphate derivatives and o-hydroxybenzaldehydes as the starting materials. All of the target compounds were characterized by IR, 1H-NMR, 13C NMR and HRMS. The optimum conditions were as following: microwaved reaction at 25℃,600W for 25min. The antitumor activity of the target compounds was determined by MTT method. The results showed that the target compounds had inhibitory effects against three kinds of tumor cells: human acute myeloid leukemia cells (KGla), human hepatoma cells (HepG2), cervical cancer cells (Hela). Among the ten compounds, 3E, 3F showed a good inhibitory activity against HepG2.
CHENG Lu , XIE Xiang , LIU Zhongyuan , SONG Shuang , LI Hong-Yan , CUI Li , ZHOU Da-Yong , JIA Jin , ZHANG Jiang-Hua
2018, 35(2).
Abstract:To develop the application of saponins from sea cucumber cooking water in the field of cosmetics, three saponin fractions S1, S2 and S3 were obtained from sea cucumber cooking water with methods including alcohol precipitation, macroporous resin absorption and ethanol gradient elution, and characterized by Infrared spectra. The contents of total saponins in obtained saponin fractions were determined by vanillin-acetic acid method. 1, 1-diphenyl-2-picrylhydrazyl (DPPH) method was adopted to measure the antioxidant activity of each fraction aqueous solution and ultraviolet spectrophotometric method was applied to determine the tyrosinase inhibitory activity, both of which comprehensively evaluated the whitening and antisenility efficacy of each saponin fraction. The results indicated that the fractions S1, S2 and S3 all contained triterpenoid saponins, mass fractions of which were 6.09%, 34.08% and 63.51% respectively. Among the three fractions, the fraction S2 aqueous solution possessed promising whitening and antisenility efficacy according to the higher DPPH free radical scavenging capacity and inhibitory action on tyrosinase activity. Specifically, when the concentrations were greater than or equal to 5 g/L, the scavenging ratios were kept at 92.5%, and when the concentrations were from 50 to 70 g/L, the inhibitory ratios were stable at 30.4%. Accordingly, this work was the continue efforts for the development of excellent cosmetic additives for skin whitening and antisenility.
2018, 35(2).
Abstract:Tetracaine hydrochloride was synthesized from N-alkylation,hydrolysis and esterification through three-step reactions,The yield of tetracaine hydrochloride was up to 85.09 %. FTIR,1HNMR and HPLC were used to characterize and analyze the structure and purity of the products.The reaction conditions were optimized, which was studied with the reaction of N-alkylation,hydrolysis and esterification. The results show that,tetracaine hydrochloride is successfully synthesized. The optimal process conditions of N-alkylation, under which the yield of ethyl 4-(butylamino) benzoate( I) is up to 75.69%, are as follows: at 60℃, and with the ratio of triethylamine, benzocaine and 1- bromobutane is 1.2:1:4.6. Compared with the present technology route,the new method has successed in reducing the formation of dibutyl by-product, during formed the key intermediate of ethyl 4-(butylamino)benzoate(I). The optimal synthesis conditions of hydrolysis, are as follows: at 50℃, and with the ratio of sodium hydroxide and ethyl 4-(butylamino)benzoate is 1.4:1. We can get the target product in 8 hours. The production of 4-(butylamino)benzoic acid (Ⅱ)with a 99.78% yield. The optimal reaction conditions of esterification, are as follows: at 116℃, and with the ratio of 2-dimethylaminoethyl chloride hydrochloride and 4-(butylamino)benzoic acid is 1.3:1. The solvent methyl isobutyl ketone ensures the production of tetracaine hydrochloride with a 85.09% yield.
ZHAO Guo-qun , JI Xiao-li , LIU Jin-long
2018, 35(2).
Abstract:Three kinds of yeast mannan with different molecular weights, namely YM-30, YM-50 and YM-90, were prepared by extracting with water in high temperature and ethanol precipitation fractionation. The weight average molecular weights, solubility, pH and viscosity of three kinds of yeast mannan were determined, and their hygroscopicity and moisture retention were investigated. The results show that the weight average molecular weights of YM-30, YM-50 and YM-90 were 12.40×104 Da, 4.47×104 Da and 2.16×104 Da respectively. YM-30 with large molecular weight was not soluble or slight soluble in water, but YM-50 with medium molecular weight and YM-90 with small molecular weight were soluble in water. YM-30 solution was weakly-alkaline and YM-50 solution was neutral, but YM-90 solution was weakly-acidic. The solutions of YM-50 and YM-90 had very low viscosity which was almost the same that of water. Furthermore, their viscosities were not influenced by mannan concentration and temperature. The infrared spectroscopy spectra showed that the polysaccharide chains of three yeast mannan were β-D-pyran type structure. Under the condition of low moisture (RH 43%), YM-90 had the strongest moisture absorbability. However, under condition of high moisture (RH 81%), the moisture absorbability of YM-30 was the best. Under the environment of RH 43%, moisture retention of YM-30 was the best, and its moisture retention ratio was 98.4%, which was slightly higher than that of hyaluronic acid. Yeast mannan from Saccharomyces cerevisiae had perfect moisturizing performance.
2018, 35(2).
Abstract:Polyacrylic acid/attapulgite (PAA/ATP) nanocomposites were prepared by copolymerization of acrylic acid and the modified attapulgite which was obtained by γ-methacryloxy propyl trimethoxy silane(KH-570) modifying. The results showed that PAA/ATP nanocomposite was successfully obtained, and the ATP in PAA/ATP nanocomposite can be uniformly dispersed. The appearance stability and thermal stability of PAA/ATP nanocomposites were the optimal when When the amount of ATP in acrylic acid(AA)was 1%. It indicated that the flame retardancy and thickening properties of the leather had improved when the PAA/ATP nanocomposite was applied to the retanning process of wet blue sheep leather. Meanwhile, the flame retardancy of the leather after the retanning of the PAA/ATP nanocomposite was the optimal when the amount of ATP in acrylic acid(AA)was 1%.
ZHANG Hao , LIU Ye , ZHANG Yi , DING Chang-kun , NIU Qianqian , ZHOU Sheng
2018, 35(2):0-0.
Abstract:With Corn starch (St), methyl acrylate (MA) and L- arginine (L-Arg) as raw materials, basic amino acids were introduced into the starch molecules by the two step of esterification and ammonolysis process ,the antibacterial modified starch (StMA-Arg) was prepared. The reaction mechanism was introduced, the structures of the products were characterized by Raman spectroscopy (RAM) and X- ray diffraction (XRD) analysis, the reaction conditions were optimized by single factor experiments. The antibacterial films were prepared by using the modified starch as raw material. The hydrophobic properties, mechanical properties, antibacterial activity and stability of the films were investigated. The results showed that the mechanical properties of StMA-Arg film were significantly improved compared with native starch film, and the hydrophobicity of the film was enhanced. StMA-Arg film showed obvious antibacterial activity to Escherichia coli, and the bacteriostatic circle was small, which belongs to contact bacteriostasis. The results of weight loss experiment showed that the weight loss rate of StMA-Arg film was 27.90% after 40D, which was much lower than that of native starch film (40D weight loss rate was 72.15%) . As a potential substrate for environmental remediation, the enhance in antibacterial activity and the degradation resistance of StMA-Arg and its films were of great significance to improving the stability of starch-type natural polymer materials, prolonging its service life and expanding its application scope, so as to realizing its industrial application in the field of environmental remediation.
2018, 35(2).
Abstract:A cyclic phosphate flame retardant named DOPC-THPE was synthesized from neopentyl glycol, phosphorus oxychloride and 1,1,1-tris(4-hydroxyphenyl)ethane (THPE). The chemical structure of DPPC-THPE was identified via FTIR, 1HNMR, 13CNMR and 31PNMR. TGA curves indicated that DPPC-THPE had good charring performance and thermal stability, with a char of 35.9% at 700 ℃. Then the product was added to polypropylene to improve its flame retardancy. Limited oxygen index (LOI) and vertical burning tests were utilized to investigate the flame retardancy of the samples. The results suggested that when the loading of DOPC-THPE was 30.0 wt%, the LOI value of PP composite could be increased from 17.5 to 25.0% and V-1 rating could be achieved.
YANG Dong-ming , SHI Xin , XU Yan-yan , ZHUO Miao , CUI Guo-dong , GUO Ji-xiang
2018, 35(2).
Abstract:According to the the characteristics of high salinity oilfield sewage collection system corrosion, using rosin and oleic acid, hydroxyethylethylene diamine and sodium chloroacetate, through amidation, cyclization and quaternization reactions, adding sodium ethylenediamine tetramethylenephosphonate, developed a corrosion inhibitor SDH-1 for high salinity. The structural characterization of the corrosion inhibitor SDH-1 was characterized by IR and GC-MS, the corrosion inhibition performance of it for 20# steel was evaluated, and it’s scale inhibition performance and demulsification performance were investigated; the inhibition mechanism was analyzed by isothermal adsorption behavior and polarization curve measurement. The results show that when the inhibitor concentration of SDH-1 was 30 mg/L, the corrosion inhibition efficiency was 90.47% in the formation water system with salinity of 243063 mg/L, the antiscale rate was 85.96%, the water diversion rate was 96.3%; the adsorption of corrosion inhibitor on the metal surface is in accordance with Langmuir adsorption isotherm, which is a kind of compound corrosion inhibitor mainly for suppressing anode corrosion . Compared with the commercially available corrosion inhibitors, the corrosion inhibition efficiency of corrosion inhibitor SDH-1 was increased by more than 12%, which could effectively reduce the corrosion rate of pipeline steel under high salinity.
2018, 35(2).
Abstract:SO42-/TiO2-SnO2 as solid acid catalyst was used for the synthesis of 1,4-butanediol acrylate with 1,4- butanediol and acrylic acid as experimental material. The effects of the mole ratio of acid to alcohol, the amount of catalyst, reaction temperature and reaction time on the conversion of 1,4- butanediol and yield of 1,4-butanediol acrylate were studied. The optimized process conditions were obtained by using response surface methodology on the based of single-factor tests. The optimized process conditions were as follow : the mole ratio of acid to alcohol of 2.62:1, the amount of catalyst of 8.88% of the total mass of 1,4- butanediol and acrylic acid, reaction temperature of 136.24℃ and reaction time of 4.68h. Considering the actual situation, the reaction temperature was trimmed about 136℃. Meanwhile, 5 groups of repeated verification experiments were carried and the average yield of 1,4-butanediol acrylate was 88.12%. By the NMR analysis confirmed that the products were 1,4-butanediol acrylate and the physicochemical indexes accord with relevant standards, especially the purity in 95%~98% and the acid value was 0.133 mgKOH/g. This was obviously better than the standards.
2018, 35(2).
Abstract:An anti-clay agent AA-SAS was synthesized by acrylic acid (AA) and sodium allylsulfonate(SAS) to improve the adverse effects of the clay for concrete. The copolymer was analyzed by IR, GPC, TG and XRD. The effect of the copolymer on the workability of cement paste and concrete with different clay was investigated. The results show that the molecular weight of AA-SAS is smaller and the diffusion rate of which is faster than polycarboxylate superplasticizer. The copolymer can be adsorbed preferentially by the clay in the concrete, thus reducing soil adsorbing polycarboxylate superplasticizer. The copolymer has a good anti effect on bentonite, kaolinite, mica and Weihe clay. The workability of concrete is improved obviously while adding the copolymer. When the solid content of AA-SAS was 0.11% of the cementing material, the 0.5 h concrete slump and fluidity is improved by 15 and 90 mm, and the 1 h concrete slump and fluidity is improved by 20 and 100 mm. In comparison with polymer(AA-AM)synthesized previously, the copolymer AA-SAS shows better property on resisting clay.
jiangxue , Liu Ke-jiang , Wang Hui-fei , JI wen-peng , HU jian , TIAN yang , ZHONG cai-ling , HU Xiang-nan
2018, 35(2).
Abstract:To synthesis the important intermediates of saxagliptin and optimize its preparation process by the central composite design-response surface methodology. It was prepared from 1-adamantanecarboxylic acid by a mixture of sulfuric acid and nitric acid to obtain 3-hydroxy-1-adamantanecarboxylic acid,then was treated with acetyl chloride , sodium diethyl malonate and AcOH/H2O/H2SO4 to get 3-hydroxy-1-acetyladamantane.In this study, the central composite design-response surface methodology was employed to optimize the reaction temperature, reaction time and the mole ratio of 3-hydroxy-1-adamantanecarboxylic acid to acetyl chloride. The overall yield of 3-hydroxy-1-acetyladamantane based on 1-adamantanecarboxylic acid reached up to 70%. The optimized route shortened the reaction time ,saved cost and improved production efficiency,which was suitable for industrial production.
LIU Yan-long , HU Zhong-yuan , FENG Wei-wei , WANG Xiao-ning , XING Lei , LIU Fei
2018, 35(2).
Abstract:Abstract: (R,E)-3-(5-((ethoxycarbonyl)amino)cyclohex-1-en-1-yl)acrylicacid(Ⅰ), the key intermediate of vorapaxar was prepared from (E)-3-(5-nitrocyclohex-1-en-1-yl) acrylicacid(Ⅱ) via esterification, reduction, chiral resolution, condensation and hydrolysis. The reaction conditions were optimized for the synthesis of I. The results showed that ethyl(R,E)-3-(5-amino-cyclohex-1-en-1-yl)acrylate was obtained with a yield of 35.6%, using D-malic acid as separation agent and V(Methanol):V(acetone)=1:1 as solvent. The total yield of this target compound was improved to 27.4%. The structure of target compound was identified by 1HNMR and ESI-MS. The improved process is facile with relatively convenient operation procedures and suitable for industrial production.
Bai Guoyi , Chu Xiaoning , Niu Libo
2018, 35(2).
Abstract:A green method for the synthesis of 4-methoxycyclohexanone was established in this paper. Catalytic hydrogenation of 4-methoxyphenol was first carried out over supported nickel-based catalysts. Subsequently, the hydrogenation solution was oxidized by hydrogen peroxide to further improve the selectivity for the target product. The influence of two kinds of preparation methods, including deposition-precipitation and impregnation method, as well as reaction conditions on the activity and stability of the catalysts for hydrogenation was investigated. As demonstrated by X-ray diffraction (XRD), H2-temperature programmed reduction (H2-TPR) and Transmission electron microscopy (TEM) characterizations, the Ni/Al2O3-DP catalyst, prepared by a deposition-precipitation method, exhibited higher dispersion, smaller particle, and stronger interaction between the active particles and the support, compared with the Ni/Al2O3-IMP catalyst, prepared by an impregnation method. These structural characters account for its superior catalytic activity and stability in 4-methoxyphenol hydrogenation. In the hydrogenation of 4-methoxyphenol, Ni/Al2O3-DP was used as catalyst. The optimum reaction conditions were as follows: reaction temperature 423 K, reaction pressure 4.0 MPa, reaction time 1 h, m(4-methoxyphenol): m(Ni/Al2O3-DP) = 6:1.The effect of the oxidation conditions was also investigated to achieve better results. It was found that the total selectivity for 4-methoxycyclohexanone can reach 95.3%, while the reaction temperature is 353 K, the reaction time is 20 h, and the ratio of n(4-methoxycyclohexanol): n(sodium tungstate): n(oxalic acid) : n(hydrogen peroxide) is 100: 1: 1: 250.
2018, 35(2):0-0.
Abstract:In this work, nanoporous sodium montmorillonite clay (Na+-MMT) was used as a support for the immobilization of various thiazolium salts. The composite catalyst was used for preparation of 1,3-dihydroxyacetone in the formose reaction. The structure and morphology of the thiazolium-MMT was confirmed by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The catalytic performance of this immobilized thiazolium salts were probed for the formose reaction. The effects of reaction time, reaction temperature, different catalysts, and the amount of composite catalyst on the yield of dihydroxyacetone were investigated. The optimized procedure as follows: the consumption of formaldehyde is 30 mmol, thiazolium- MMT catalyst is 1.35 g, at 120 ℃ reaction 30 min, the yield of DHA is 62.3%. Also, this catalyst can be reused three times with satisfied catalytic activity.
2018, 35(2).
Abstract:A phosphorus-nitrogen flame retardant curing agent phenyl phosphonic m-Xylylene diamine diamide(PPMXD) was synthesized by phenylphosphonic dichloride(PPDC) and m-Xylylenediamine (MXDA), The chemical structure of the obtained compound was identified by FT-IR、1HNMR、ESI-MS. The thermal stability of PPMXD was tested by DSC and TG. The effects of mole ratio of reactants, reaction temperature and time, the solvent dosage and the type of solvent were investigated. The experimental results demonstrated that the yield of PPMXD was maximum when the reaction temperature was 20℃, the reaction time was 7h, n(PPDC):n(MXDA)=1:3.5, methylene chloride and N,N dimethylformamide was used to be mixed solvent which quantity ratio of methylene chloride to N,N dimethylformamide was 2.3:1, m(solvent):m(PPDC)=12:1. The PPMXD was used in epoxy, TGA and SEM would study the thermal properties and the epoxy resin carbon residue morphology. The flame retardant properties of epoxy resin were tested by limiting oxygen index (LOI) and vertical experimental characterization of the combustion. When the addition of PPMXD was 28.5%, it could through the UL-94 V-0 test, the oxygen index could reach 29%, the tensile strength and impact strength could reach 42.89MPa and 6.45KJ/m2, respectively. The results of TGA showed that compare with EP, the addition of PPMXD could make the largest thermal decomposition rate of EP2 decrease from 18.93%/min to 13.28%/min, at the same time, the amount of residual carbon at 800℃ also increased from 16.12% to 18.86%. The SEM results show that the surface of the epoxy resin after buring was rough and foamed obvious, which performed good flame retardancy.
2018, 35(2).
Abstract:The polyelectrolyte membrane was prepared by interaction between chitosan (CS) and acacia(GA) using glutaraldehyde as linkage reagent, glycerol as plasticizer. The property such as water resistance and tensile strength were studied using single factor analysis. The optimal formula for determining the composite film to determine the better formula of the membrane. FTIR was applied to analysis the function groups of the bipolar membrane. SEM was used to observe its surface structure. XRD was used to analysis the compatibility of membrane components.The results showed that the polymer film has good compatibility, and contains - COOH, - NH3 functional groups with the characteristics of the gender, the film can be stable in acid and alkali solution. The structure and properties were studied and the membrane was a separator in the electrolysis cell to produce thioglycolic acid (TGA). The experimental results showed that thioglycolic acid was prepared effectively by electro-reduction of dithioglycollic acid blended with thioglycolic acid in the cathode room and 25% H2SO4 as the anode electrolyte1.The current efficiency was up to 71.77% at room temperature when current density was 10 mA/cm2