gengyanru , dingjing , huanglongjiang
2019, 36(3).
Abstract:According to the structural characteristics of compounds containing 1,2, 4-triazole moiety, the research progress on antiepileptic activities of fused heterocyclic and non-fused heterocyclic compounds is summarized. The relationship between different structural types with antiepileptic activities and neurotoxicity is emphatically analyzed. It is concluded that 1,2,4-triazole fused quinoline derivatives, quinazoline derivatives and triazole thione derivatives are valuable for further research and development due to their good activity and low toxicity. Finally, the future research directions of 1,2,4-triazole derivatives with antiepileptic activity are prospected.
QI Xiao-hua , JIANG Jin-yun , LV Lu , LI Chuan-qiang , GUO Chun-wen , MOU Yuan-hua
2019, 36(3).
Abstract:A γ-polyglutamic acid/attapulgite superabsorbent composite was prepared using γ-polyglutamic acid and attapulgite as materials, and polyethylene glycol glycidyl ether as crosslinking agent. The structure and surface morphology of the superabsorbent composite were characterized by Fourier transformation infrared spectroscopy (FTIR) and scanning electron microscope (SEM). The effects of the mass fraction of γ-polyglutamic acid and attapulgite, pH value of solution, the mass fractions of NaCl, ZnCl2 and Na2SO3 on the swelling ratio were investigated in distilled water. The results showed that the suitable mass fraction of γ-polyglutamic acid and attapulgite were 14% and 6%, and the suitable pH value was 5~9. The lower the mass fraction of the ions in the solution, the greater the swelling degree of the superabsorbent composite. ZnCl2 aqueous solution had a great influence on the swelling behavior of γ-polyglutamic acid/attapulgite superabsorbent composite. In addition, the superabsorbent composite had good water retention.
2019, 36(3).
Abstract:A family of double-network hydrogels were prepared by copolymerization of acrylamide(AM) with three carboxyl acid-based monomers, acrylic acid (AAc), itaconic acid (IA) and maleic acid (MA), via a combination of chemical cross-linking and soaking in aqueous solution of metal cations. The structures of the hydrogels were characterized by SEM, the coordination forms of carboxyl group with metal ions were analyzed by FT-IR and TGA, the effective network chain density and molecular weight of the chain length between cross-linking points were evaluated using rubber elastic theory, and the effects of carboxyl acid-based monomers and multivalent cations on mechanical properties of the obtained hydrogels were investigated using electronic tensile machine. It was revealed that the single chemical cross-linked hydrogel had uneven interconnection structures with tensile strength of 3.3 kPa. After soaking in divalent cations such as Ca2 , Fe2 and Cu2 , the –COO- groups formed bidentate coordination, resulting in an increase of tensile strengths to 43, 54 and 22 kPa for Ca2 , Fe2 and Cu2 , respectively. In contrast, –COO- groups formed the chelation-bridging tridentate coordination with Fe3 . So the hydrogel after soaking in Fe3 had the highest thermal decomposition temperature and densest structure. As a result, tensile strength increased to 6123 kPa. In addition, tensile strength of hydrogels by copolymerizing AM with AAc and IA were higher than 4.0 MPa while that copolymerized with maleic acid were only around 1.0 MPa. The introduction of ionic bonds between Fe3 and –COO- not only improves the mechanical properties of the hydrogel, but also endows it with self-healing properties. The tensile strength of healed gel can reach 130 kPa.
MA Rui-ying , MA-Di , 赵晓霞 , XU Guang , WEN Ping , ZHANG Ying
2019, 36(3).
Abstract:NH2-MIL-125(Ti) crystals were prepared by a solvothermal method. By varing the ratios of N,N-dimethylformamide (DMF) and methanol (MeOH) in the synthesis system, NH2-MIL-125(Ti) crystals exhibited circular plate, decahedral or octahedral morphology. XRD, SEM, FT-IR and BET characterization techniques were used to study the physical properties of NH2-MIL-125(Ti) crystals with different morphologies. Then these crystals were used in the photocatalytic oxidation of cyclohexane under visible light irradiation. The structure-activity relationship between catalytic performance and crystal plane was explored. Results showed that the main reaction of selective oxidation of cyclohexane to target products cyclohexanol and cyclohexanone occurs in the {110} crystal face family of NH2-MIL-125(Ti) crystal, whereas the {101} crystal face family is mainly to further oxidize cyclohexanol and cyclohexanone into COx.
WANG Rui-ping , YU Huang , YUAN Chang-long , WANG Jia-sheng , TANG Fang-cheng , TAO Jing-song
2019, 36(3).
Abstract:In order to solve the problem of high expansion coefficient and poor thermal stabilityof the flexible organic solar cellsubstrates, this paper proposed a method that using cellulose nanofibrils to reinforce epoxy resin as the flexible substrate of organic solar cells. In this paper, the nanocellulose with highly transparent and outstanding thermal stability properties were took to improve the epoxy’s thermal stability that possesses high thermal expansion coefficient, therefor a new nanocomposite substrate material is achieved by preparing a transparent film of nanocellulose impregnated with epoxy resin. The results shown the thermal expansion coefficient of composite film decreases from 46×10-6/K to 19×10-6/K comparing with the pure epoxy resin, and the new substrate also has outstanding light transmittance(89%), smooth surface (roughness 2.15nm), good mechanical properties (Young'smodulus 2.3GPa, tensile strength 59MPa). According to this results, a poly(3,4-ethylenedioxythiophene):polystyrene sulfonate conductive electrode was deposited on the nanocomposite substrate and the surface morphology and conductivity were performed between -15°C to 70°C. The results proved that electrode materials deposited on the substrate hadn’t any crack when the temperature changed, and the conductivity remained stable (830-875S/cm).
2019, 36(3).
Abstract:Polyoxypropylene glycol (PPG),bihydroxy hydrophilic polysiloxane polyol(UC3667) as the soft segment,isophoronediisocyanate (IPDI), 1,4-butanediol (BDO), dimethylolpropionic acid (DMPA) and ethylenediamine (EDA)as the hard segment,a series of waterborne polyurethanes(WPUs)were prepared based on polysiloxane.The effect of polysiloxane on the particle size and stability of waterborne polyurethanes emulsion was investigated by Malvern laser particle size analyzer. The structure of waterborne polyurethane was characterized by infrared spectroscopy (FTIR), and the tendency of silicone to move to the surface of the film was analyzed. The thermal stability, mechanical properties and surface properties of waterborne polyurethane films were characterized by thermogravimetric analysis, contact angle and X-ray photoelectron spectroscopy. The results showed that when the content of polysiloxane increased, the tensile strength of waterborne polyurethane films increased firstly and then decreased; and the introduction of polysiloxane improved the thermal stability, elongation at break, contact angle of waterborne polyurethane films and reduced surface energy. Whenthe content of polysiloxane is 5.0%,polysiloxane migration on the surface of the film reached saturation, and the surface energy is 27.27 mJ/m2.
PANG Jin-ying , HUANG Chun-yan , LAN Chun-bo , TAN Deng-feng , MO Xian-zhong , LIU Yu-xin
2019, 36(3).
Abstract:The banana microcrystalline cellulose was prepared by the banana fiber, and the esoporous materials were prepared by the mecobalamin, banana microcrystalline cellulose and PLGA. The esoporous materi-als were characterized by SEM, specific surface area and pore size analysis (BET), Thermogravimetric mass spectrometry (TG-MS) and FT-IR. The drug load content, encapsulation efficiency, and in vitro re-lease rate of mesoporous materials loading mecobalamin were studied by the UV spectrophotometry. FT-IR spectrum analysis showed that the main component of microcrystalline cellulose was cellulose. The BET results showed that the average pore diameter [4V(pore volume)/A(surface area)] of banana micro-crystalline cellulose/PLGA mesoporous materials loading mecobalamin was 17.89nm. TG-MS results showed that the decomposition temperature of the materials were about 300℃. The results indicated that the materials had great control release ability, the drug release following zero-order release kinetics.
YANG Jian-zhao , SUN Hong-juan , PENG Tong-jiang , YUE Huan-juan , LEI Dei-hui
2019, 36(3).
Abstract:Graphene oxide (GO) with different oxygen-containing functional groups was prepared by improved Hummers method, then ultrasonic dispersion. And the graphene oxide film prepared by spin coating method. The type and content of the functional groups, spectral characteristic were implemented by XRD, FT-IR, XPS. Ammonia(NH3) sensitivity is tested by WS-30A gas sensing system. The result shows that graphite oxide contains oxygen functional groups such as hydroxyl group (C-OH), epoxy group (C-O-C) and so on, the maximum spacing of surface network reaches 0.935 nm;with the oxidation degree increases, the initial resistance of the component increases from 550 KΩ to 2500 KΩ. The sensitivity of different GOs gas sensors to NH3 is positively correlated with the relative content of hydroxyl group. When the relative content of hydroxyl group in GOs is 43.75%, the maximum sensitivity of gas sensor to 80 ppm NH3 is up to 78%, and the response time is 37 s, and the gas sensor exhibits good stability and repeatability, the minimum error of repeatability is 3.1%. There are two mechanisms for the response of GOs to NH3 molecules: the ionic conductance mechanism of NH3 molecules entering GOs interlayer water molecules after hydrolysis to form NH4 ions; the charge transfer mechanism of hydrogen bonds formed by oxygen functional groups on the GOs structure layer after adsorbing NH3 molecules.
SU Xiuxia , ZHANG Rong , HE Shengzhuo
2019, 36(3).
Abstract:A waterborne nitrocellulose (PWNC) emulsion modified by Polyacrylic grafting copolymerization was prepared by selfemulsification with nitrocellulose(NC) 、acrylic acid(AA) 、hydroxypropyl acrylate(HEPA) and hexamethylene diisocyanate(HDI) as main raw materials. Then, the corresponding PWNC films were obtained. Fourier transform infrared spectroscopy (FTIR), contact angle measuring instrument, transmission electron microscope (TEM), thermal gravimetric analyzer (TGA) and nano particle surface potential analyzer were use to characterize the chemical structure, hydrophobicity, particle morphology, thermal properties of PWNC films and the particle size of PWNC emulsions. The effects of dosage of DBTDL, mole ratio of AA to HEPA on the properties of emulsion and film were also studied. The results showed that the PWNC emulsion was stable and the particles of emulsion were regularly spherical with a core-shell structure. When the mole ratio of AA to HEPA to HDI was 3∶1:0.75 and the NC was 3.6g, the PWNC emulsion exhibited smaller particle size and narrow particle size distribution. Theaverage particle size and polydispersity index(PDI) were 52 nm and 0.021. respectively. The contact angle of modified PWNC films increased to 122.5? , Which indicated that the modified PWNC films had better water resistance than the NC films.
Zhang liming , Liu zhanli , Wang xiangyou , Sun yang
2019, 36(3):0-0.
Abstract:Abstract: The blend solutions (C/Z-0、C/Z-1、C/Z-3、C/Z-5) with different mass ratios of chitosan and zein and then according blend films were prepared by solution casting method. The effects of mss ratios on rheological properties of blend solutions, microstructure and thermal properties of blend films were analyzed by rotational rheometer, SEM and DSC. The results showed that the blend solutions of different ratios all had pseudoplastic properties. With the increase of zein content, the consistency coefficient decreased, and the fluid index increased from 0.849 to 0.882. The activation energy of blend solutions increased gradually. The dynamic frequency scanning rheological analysis showed that the storage modulus and loss modulus were dependent on frequency. With the increase of zein content, both values increased, and the crossing point moved towards the low-frequency, which indicated the intermolecular hydrogen bonds was enhanced. In C/Z-1 blend films, chitosan and zein molecules bound tightly and had good compatibility, which also leaded to the improvement of thermal stability of blend films.
ZHANG Yu , XIN Lu , ZHANG Luqi , JIAO Xuejuan , HU Yazhuo , LIU SHuting , SUN Jie , WANG Miaomiao , ZHANG Baohua
2019, 36(3):0-0.
Abstract:Using chitosan and sodium alginate as raw material and 4A zeolite as structural modifier, 4A zeolite/sodium alginate/chitosan composite microspheres were prepared by complex condensation, the composite microspheres were characterized by means of microscope、SEM 、XRD and FTIR. The effect of 4A zeolite on microsphere formation and swelling properties of the composite microspheres was investigated. The results show that the weight and particle size of the composite microspheres increased with the increase of the 4A zeolite addition. 4A zeolite was beneficial to the granulation of Composite Microspheres, The highest rate of granulation reached 98.5%. After freeze-drying, the particle size were uniform, and the sphericity was regulation. Under different pH and temperature conditions, 4A zeolite can effective inhibits the swelling performance of composite microspheres, but the microspheres still maintained pH and temperature sensitivity. 4A zeolite can be used as a structural modifier in drug controlled release system for further research and application.
2019, 36(3):0-0.
Abstract:Graphite oxide (GO) dispersion liquid was prepared with graphite, concentrated sulfuric acid, potassium permanganate and hydrogen peroxide as main raw materials and by Hummers method. Then GO powder was obtained by freeze drying of GO dispersion liquid. The polypropylene (PP)/GO composites were prepared by mixing of melt PP and GO powder. The microstructure and performances of GO and PP/GO composites were characterized using various testing methods such as FTIR, AFM, TEM, XRD, DSC and conductometer as well as oxygen index determinator. The results indicated that the GO can uniformly distribute in the PP matrix with double layers result in forming compact and even microstructure in PP/GO composites. The mechanical properties, heat-resistant property, flame resistance and thermal conductiveof PP/GO composites have a significant improving compared with the control sample (pure PP resin). When GO dosage is 0.4% by PP mass, the tensile strength, flexural strength and impact strength of the GO/PP composites have an increase rate of 29.6%, 33.6% and 62.7% compared with the control sample, respectively. Meanwhile, its melting point increase to 174.2℃ from 154.5℃, and its thermal conductivity has an increase rate of 205.3%, and the limiting oxygen index increase to 27.6 from 18. The research results indicated that the performances and application fields of PP will be improved by forming composites with GO nanosheets.
ZHANG Xiu-juan , JIA Xu , ZHANG Yue-jun , TAO Xian-ping
2019, 36(3).
Abstract:Poly(N,N-diallyl-N-methylpropylammonium chloride)(PMPDAAC) was prepared by N,N-diallyl-N-methylpropylammonium chloride (MPDAAC) as monomer and 2’2-azobis(2-methylpropionamidine) dihydrochloride (V50) as initiator in aqueous solution. On the basis of single factor experiments, the Box-Behnken mathematical relational model between the intrinsic viscosity values of PMPDAAC and their affecting factors was established, and the preparation conditions of PMPDAAC were optimized. The optimum preparation conditions were: T1=56.13℃, T2=61.24℃, T3=80.22℃, w(MPDAAC)= 71.03%, w(V50)= 2.50% and w(Na4EDTA)= 0.0074%, the average value of intrinsic viscosity of PMPDAAC and conversion rate of monomer under optimal conditions reached 1.17dL/g and 92.05%, respectively. The structure of the product was characterized by FTIR and NMR, and its Mw and polydespersity d(Mw/Mn) was measured by GPC-MALLS. The results showed that the maximum Mw of the product PMPDAAC was 2.658×105, polydespersity d(Mw/Mn) was 1.358. The research showed that the space effect and possible solvent effect brought about by the substituent propyl group were the main factors affecting the polymerization activity of diallyl quaternary ammonium salt.
2019, 36(3):0-0.
Abstract:A pH-responsive amino acid amphoteric surfactant —— N-lauryl-(α-methyl)-β-aminopropionate (AAS-1) was synthesized by a two-step reaction using dodecylamine and methyl methacrylate. The synthesis conditions were optimized by single factor experiments. The optimal synthesis conditions were as follows: n(dodecylamine):n(methyl methacrylate)=1.0:1.4, and the reaction temperature was 60 ℃, and the reaction time was 10 h. For comparison, N-lauryl-β-aminopropionate (AAS) was prepared in the same way. The structures of products were characterized by FTIR and 1HNMR. The surface tensions of AAS and AAS-1 under different pH were measured by surface tension meter, and the surface tension curves was acquired, and the effect of α-alkyl on its surface activity was investigated. The foam properties of AAS and AAS-1 under different pH were studied by Waring Blender method. The results shows that AAS and AAS-1 all have pH responsiveness. Affected by α-alkyl, AA-1 has a foam volume (V0) of up to 523 mL and a foam half-life (t1/2) of up to 6.25 min when pH<7, but when pH>7, V0<125 mL, t1/2=0 min. This means that, in the acidic aqueous medium, AAS-1 has good foaming ability and good foam stability but can be defoamed quickly in alkaline water medium, which is exactly the opposite of AAS foaming regularity. It can be used as a foaming agent in the foam acid system and can be repeatedly foamed and defoamed.
2019, 36(3):0-0.
Abstract:A sulfonate Gemini surfactant N,N'-dipalmitoyl group(DS16-P-16) was synthesized by substitution and acylation reaction with the main raw materials of p-phenylenediamine, palmitoyl chloride and sodium 2-chloroethyl sulfonate, and the intermediates and target products was identified by FT-IR and 1H NMR. The water solubility, surface&interfacial activity, foaming properties and emulsifying properties were also investigated. The results showed that the structure of the synthesized intermediates and final products was consistent with the design, which confirmed that the synthesized sulfonate Gemini surfactant was the target product. The critical micelle concentration (CCMC) of DS16-P-16 was 5.01×10-4 mol/L at 25 °C,which was 6.26 percent of the traditional twelve sodium alkyl sulfonatesurfactant (SDS; 25℃,8×10-3 mol/L), the surface tension (γcmc at the critical micelle concentration is 31.9mN/m, which was 6.1 mN/m lower than SDS,showing good surface activity, pC20 (the negative logarithm of the concentration of DS16-P-16 solution required to reduce the surface tension of water by 20 mN/m) is 3.61, which is 1.1 higher than SDS, showed a better ability to reduce water surface tension;With the increase of experimental temperature and solution concentration, the interfacial tension of DS16-P-16 solution gradually decreased, and both were lower than 10-2 mN/m. At 45 °C, 0.5 percent of DS16-P-16 solution could reducethe oil-water interfacial tension to 1.46×10-2mN/m;The initial foaming height of 0.1% DS16-P-16 solution is 28 cm, the foam stabilization rate can reach 93%, and the stable time of emulsion is 437 s. Under the same conditions, the initial foaming height of 0.1% traditional surfactant sodium dodecyl sulfate (SDS) is 15 cm, the foam stabilization rateis 60 and the emulsification time is 128s.
ZHU Long-bao , YANG Jing , GE Fei , TAO Yu-gui , SONG Ping
2019, 36(3).
Abstract:In order to synthesize high value-added β-phenylalanine, the phenylalanine aminomutase was used to convert α-phenylalanine to β-phenylalanine. The phenylalanine aminomutase gene (pam) from Pantoea agglomerans was cloned, the expression vector was constructed for heterologous expression. The results showed that the gene pam with1626 bp encoding 541 amino acids of PaPAM was successfully cloned. The expression vector pET28a-pam was constructed and transferred into E. coli BL21 for induced expression using isopropy-β-D-thiogalactoside (IPTG). The electrophoretically pure recombinant phenylalanine aminomutase (PaPAM) was produced by affinity chromatograph. The product of β-phenylalanine was detected using MS and NMR. The enzyme activity reached 2.5 k U/g under the optimum conditions of 30 ℃, pH 9.0 and 1.5 mol/L NH4+.The enzyme exhibited high stability at 30 ℃~50 ℃ and pH 8~10. Metal ions and surfactants have different effects on enzyme activity. Na+, Mg2+, Ca2+, and Fe3+ have little effect on PaPAM activity, while SDS and Triton 100 can strongly inhibit activity. Under optimal condition, the conversion rate of α-phenylalanine was reached 92 %.
XUE Hong-kun , TAN Jia-qi , WANG xin
2019, 36(3).
Abstract:Changes in (total polyphenols and anthocyanins) contents, antioxidant capacity and anticancer effect, anthocyanins composition of blueberry extracts before and after in vitro digestion were investigated, and the degradation pathway of anthocyanins was speculated. Folin-Ciocalteu and pH differential methods were employed for determining the contents of total polyphenols and anthocyanins, respectively. The antioxidant capacity of the extracts before and after in vitro digestion was evaluated by the inhibition rate of liposomes, scavenging abilities on 1,1-diphenyl-2-picrylhydrazyl (DPPH) and ABTS+ radical. Anthocyanin composition was analyzed using HPLC-EIS-MS/MS based on molecular mass and fragment ions, peak sequence and related literature data. The results indicated that after in vitro digestion the content of total polyphenols increased by 47.21% while anthocyanins decreased by 71.82%, and the inhibition rate of liposomes, scavenging rate of DPPH and ABTS+ free radical increased by 38.45%, 29.41% and 29.12%, respectively, and the growth inhibition of HepG2 hepatoma cells, A549 lung cancer cells and Hela human cervical cancer cells increased significantly, and the number of anthocyanins decreased from 12 to 9. Taken together, after in vitro digestion, blueberry extracts had increased total polyphenols, antioxidant activity and inhibition of the growth of the above three kinds of cancer cells, reduced anthocyanin contents and compositions. Speculation on the degradation process of gastrointestinal anthocyanins was found that the process of degradation of cyanidin-3-glucoside to form quercetin was similar to that of pelargonidin-3-glucoside degrading kaempferol.
2019, 36(3).
Abstract:We used multienzyme coupled catalysis to produce L-Tyrosine(L-Tyr). In this study, Glycine was catalyzed to synthesize D-Serine by Aldolase(ALD), and D-Serine was transferred to pyruvic acid ammonium by D-Serine Dehydratase(SDH). Then, L-Tyr was synthesized by Tyrosine Phenol-Lyase(TPL) when the substrate phenol was added into the reaction system.The optimal reaction conditions were shown as follows: pH=8.5, 35 ℃, 6 g/L of ammonium acetate, 0.1 g/L of PLP, m(ALD):m(SDH):m(TPL)=6∶3∶5. We used the above conditions to catalyze glycine at the concentration of 50 g/L for 11 h, the concentration of L-Tyr was 117 g/L with a conversion of 97%, increasing by 4% compared with small-scale test and the yield reached 85%.The method of biosynthesis of L-Tyr can not only eliminate the purification process of D-Serine and pyruvic acid ammonium, but also has a reference significance for the reasonable utilization of resources and green synthesis process.
LEI Lei , ZHANG Wei , LIU Long , YU Xiao-dong , XIN Xiao-li , TIAN Ge
2019, 36(3).
Abstract:The technology of saponins extracting from quinoa husk using ultrasonic-complex enzyme assisted and its antioxidant activities have been established in this research. Taking the extraction rate of quinoa saponins as the index, the effects of four operational factors, that is, the ratio of cellulose and pectinase, temperature, pH value and hydrolysis time have been studied by single factor experiments. On the basis of the single factor experiments, the extraction technology of saponins from quinoa husk using complex enzyme synergistic ultrasound was optimized by response surface methodology. The optimum conditions were as follows: total enzyme dosage ( the quality of saponins as the base)was 1.5%, enzyme ratio〔m(cellulase):m(pectinase)〕 was 3∶2, enzymatic hydrolysis temperature was 50.5 °C, pH was 5.5, and enzymatic hydrolysis time was 0.25 h. Under optimal conditions, extraction rate of quinoa saponins was highest and reached 85.32%. The extraction rate using ultrasonic-complex enzyme assisted was 4.41% higher than only cellulase (81.56%), 3.66% higher than only pectinase (82.20%), and 16.76 higher than only ultrasonic extraction. The antioxidant activities of the extracted saponins was evaluated by DPPH•. The results show that the saponins obtained from quinoa husk had antioxidant activities. saponins' concentrations and antioxidant activity were in a dose- dependent manner.
2019, 36(3).
Abstract:Twelve Pyridinyl-4,5-2H-isoxazole Heterocyclic derivatives were synthesized from 2-chloro-5-chloromethylpyridine and their structures were characterized by 1HNMR, 13CNMR, MS and IR. The antibacterial activities results indicated all of them exhibited potent activities against Staphylococcus aureus (ATCC25923), Streptococcus pneumonia (ATCC49619) and Enterococcus faecalis (ATCC29212). Among of them, compound 9f and 9l showed the best activities. All the target compounds displayed excellent anthelmintic activities and the effects of compound 9a-b and 9g-h were much better than albendazole. This work provided a preliminary basis for developing novel antibacterial and anthelmintic agents. The further study on optimizing activities and mechanism-of-action is under investigation.
2019, 36(3).
Abstract:Caffeyl valine ethyl ester, caffeoyl leucine ethyl ester, caffeoyl methionine ethyl ester, and caffeoyl tyrosine ethyl ester were synthesized by using L-amino acid ethyl ester hydrochloride and caffeic acid as raw materials in the presence of a catalytic amount of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide-hydrochloride (EDC) and 1-hydroxybenzotriene (HOBt) . The structure of the product was identified by mass spectroscopy (MS), nuclear magnetic resonance (1H NMR) and Fourier transform infrared (FTIR) spectroscopies. Then, antioxidant activity and irritation were carefully measured by the DPPH free radicals scavenging, hydroxyl radical scavenging experiments and erythrocyte hemolysis experiments. Four of N-caffeoyl amino acid ethyl esters were synthesized with yields between 75% and 82%. The results showed that after the combination of caffeic acid and amino acid, all the four products showed good inhibition of DPPH free radical and hydroxyl radical activity; caffeoyl valine ethyl ester had the strongest ability to scavenge DPPH free radicals, and its IC50 value was (11.23 ± 0.24) μmol/L; caffeoylmethionine ethyl ester has the strongest ability to scavenge hydroxyl radicals, and its IC50 value is (0.24 ± 0.002) mmol/L. The three caffeoyl amino acid ethyl esters are less irritating to the erythrocyte membrane relative to the caffeic acid monomer. N-caffeoyl amino acid ethyl esters derivatives are more effective than Vitamin C and might serve as new potent antioxidant.
FU Ying , HUANG Xin , SU Man-man , DI Yong
2019, 36(3).
Abstract:A new coagulant, poly-Ti-Fe (M-PTF), was prepared using a solid “waste acid filter cake (WAFC)” derived from production process of titanium dioxide. The microscopic characteristics of M-PTF were characterized with SEM, XRD and FTIR, respectively. And coagulation performance and sludge properties of M-PTF in treating a domestic wastewater was studied using Jar tests and Fluorescence Microscope (FM), compared with that of Poly Aluminum Chloride (PAC). The results showed that M-PTF surface morphology was composed of irregular and crystalline-like structures, and appeared to be rough and polymorphous networks having larger surface area. M-PTF gave higher 29% organic matter (Chemical Oxygen Demmand, CODCr) removal than PAC at dosage 2 mmol/L, and had far greater sludge settling rate at starting point (44 mL/min) than PAC (4 mL/min). M-PTF sludge was a sort of fluffy and close-ly-connected catkins-like/cotton-like images with well-defined boundary and lower water content, while PAC almost appeared to be a sort of transparent loose flocs without well-defined boundary. M-PTF sludge volume was much smaller than PAC and the water content of M-PTF sludge was lower 1.11%~2.41% than that of PAC, corresponding to its sludge reduction of 71.28%~84.38% based on the sludge volume of PAC, largely beneficial to subsequent concentrating and dewatering.
2019, 36(3).
Abstract:The composite material was first synthesized by Na-bentonite(Bent) intercalated with hexadecyl trimethyl ammonium bromide(CTMAB)、cationic polyacrylamide(CPAM) through two-step wet method. The composition、morphology and structure characteristics were analysed by XRD、FESEM、IR、BET and TG-DTG-DSC,and it was used to absorb simulated phosphorous wastewater. The results indicated that CPAM was intercalated into the lamellar structure of Na-bentonites steadily, the layer spacing was significantly increased,the infrared spectrum showed obvious carbonyl absorption peaks, the specific surface area of the sample decreased and surface hydrophobicity was enhanced after intercalation. The results of adsorption of phosphorous wastewater showed that the order of adsorbability was: CPAM/Bent > CTMAB/Bent > Bent, with the increase in reaction temperature、the initial concentration of phosphorous wastewater and the decrease of pH value, the removal rate of phosphorus with CPAM/Bent was gradually increased. While in the condition of initial concentration of 3.5 mg/L、pH of about 5、temperature of 35 ℃、adding amount of 0.5 g/100 mL, the removal rate of phosphorus were 75 % after twenty minutes. After five times adsorption and regeneration, the adsorption ability of CPAM/Bent to phosphorus decreased significantly. The adsorption isotherms could be described by Langmuir and Freundlich equations, The adsorption process could be better satisfied with the pseudo-second order kinetic equation.
ZHOU yan , PU xiao-lin , LIU lu , WANG lei
2019, 36(3):0-0.
Abstract:In view of the current domestic problems of fewer types of polymer fluid loss additives for oil-based drilling fluids. Choosing Acrylamide(AM)、Stearyl methylacrylate(SMA)as reaction monomers, 2-methylpropionitrile(AIBN)as initiator, Divinylbenzene(DVB)as crosslinker. The oil based fluid loss additive was synthesized by dispersion copolymerization. Single factor method is used to determine the best synthetic condition of fluid loss additive. Through measure the APT filtrate losses determine the monomer ratio of AM:SMA=1:3, the monomer concentration is 5%, the crosslinker concentration is 2%, the initiator concentration is 0.7%, V(methanol):V(H2O)=7:3, the stabilizer concentration is 4%, polymerization temperature is 70℃, polymerization time is 6h. Fourier transform infrared spectroscopy shows that the structure of the product is consistent with the design, the glass transition temperature is 110℃ through DSC measure. When the dosage of fluid loss additive is 3%, the API fluid loss is 1.6mL, HTHP fluid loss is 7.2mL,The high-temperature aging test show that the fluid loss additive has the temperature resistance of 160℃. the result show that the synthesized product has better performance as oil based fluid loss additive than asphalt and have no effect on drilling fluids’ rheology, and the quality of mud cake is better than the asphalt under the same dosage.
SU Yu , Dai Yongqiang , Liao Bing , Mai Yuliang , Gao Min , Zhang Lei
2019, 36(3).
Abstract:A polycarboxylate type superplasticizer (PC) was synthesized by water solution polymerization using itaconic acid polyethylene glycol ester (IAPEG), acrylic acid (AA), maleic anhydride (MA) and sodium methylacryl sulfonate (MAS) as monomers and ammonium persulfate as initiator. The structure of copolymer was characterized by FT-IR. The molecular weight and the distribution of copolymer was characterized by GPC. And the influence of reaction condition on properties of polycarboxylate type superplasticizer were discussed. The results showed that the optimal reaction conditions are as follows: the molar ratio of IAPEG to MA to AA to MAS is 1.5:4:6:3, the dosage of initiator is 10 % according to the mass of all monomers, the reaction temperature is 80℃, the reaction time is 5h. The polycarboxylate type superplasticizer synthesized under the optimum conditions can reduce the surface tension of the solution, promote the dispersion of cement particles and make the fluidity of cement paste better. The water reducing ratio of concrete is 39.2%, The compressive strength ratio of the concrete can reach 191.4%at 7d and 154.7%at 28d respectively.
Yang Na , Zhang Hua , Hu Jing , Wang Gong-ying , Deng Zhi-yong
2019, 36(3).
Abstract:As an important biomaterial platform molecule, ethanol has become a multi-functional raw material for synthesis of high value-added chemicals. The catalytic performance of various metal halide as catalysts were studied for one-step liquid phase synthesis of 1,1-diethoxyethane (DEE) by oxidation of ethanol. Among them, When RuCl3 was used as catalyst, the catalytic performance was best. Also the influence of the amount of RuCl3, reaction pressure, reaction temperature, reaction time and stirring speed on the performance of oxidation of liquids ethanol to 1,1-diethoxyethane. When the amount of ethanol is 50ml, under the optimized reaction conditions (0.01gRuCl3,2MPa,120℃,3h and 600r/min), the conversion of ethanol reached 38.2% and the selectivity of DEE reached 78.9%.This is because that Ru3+ has good catalytic performance for the oxidation of ethanol to aldehyde, and RuCl3 is a Lewis acid which can promote the condensation of ethanol and acetaldehyde. Last the recycle performance of RuCl3 was investigated, after reused 20 times, RuCl3 catalyst still has good performance.
WANG Xuan , JIANG Xiao-Hui , YU Liang-Min , ZHU Li-Wei
2019, 36(3).
Abstract:Aromatic hydrocarbons and N-Hydroxymethylacetamide were used as raw materials, seven new acetamide containing capsaicin moieties (A, B, C, D, E, F, G) were synthesized via Friedel-Crafts alkylation reaction and their structures were confirmed by IR and 1H NMR. The bioassay results showed that all the seven compounds exhibited good inhibitioneffect against Staphyloccocus aureus, Escherichia coli, Phaeodactylumtricornu- tum, Skeletonemacostatum and Chaetoceroscurvisetus. In particular, compound G had the best inhibition effect, the minimal antibacterial concentration was 0.0625 mg/mL, and the inhibition rate was over 90% at 3 mg/mL.