2018, 35(10).
Abstract:To optimize the formulation of S( )-IBU/acid-MMT dry suspension by the central composites design-response surface methodology. Using surface area and pore volume as indexes, the influence of hydrochloric acid concentration; reaction time and temperture was investigated by central composite design-response surface method. The results were fitted by second-order polynomial equation, and the optimal preparation technology was predicted according to formulation. The quality of S( )-IBU/acid-MMT composites were characterizedby powder XRD and SEM. Central composite design finalized prescription is 3.3 mol/L, 5.5 h, 55 ℃, its BET surface area and pore volume is 318 m2/g, 0.51 cm3/g, respectively.The acid-MMT loading capacity 460.8 mg/g. Using the central composite design-response surface method to optimize the preparation of S( )-IBU/acid-MMT dry suspension has a good prediction S( )-IBU/acid-MMT dry suspension showsmore capacity by central composites design.
GONG Jia-yang , XU Hai-ming , LI Dong-ya , SUN Jing-yu , XIA -Dong-sheng
2018, 35(10).
Abstract:The Bi2O2CO3 photocatalyst was successfully synthesized by hydrothermal method using urea as surfactant. X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), selective electron diffraction (SAED) and UV-visible diffuse reflectance spectroscopy (DRS) techniques were used to investigate the Bi2O2CO3 products. The results showed the size of Bi2O2CO3 samples was less than 2 μm, and absorption edge of the samples prepared using 0.1 g urea as surfactant is 394 nm and the band gap is 3.14 eV. Sample prepared by 0.1 g urea had excellent photocatalytic activity. The results showed: RhB was degraded by 20% under visible light for 200 min, and the degradation rate of RhB was 80% at 120 min under UV light, which was higher than TiO2. Superoxide radical (O2-) and the hole (h ) are the main active species in the photocatalytic degradation of Bi2O2CO3. Cyclic degradation experiments showed that the synthesized samples had high stability.
2018, 35(10).
Abstract:Surfactant flooding used in tertiary oil recovery is a kind of crucial method for stable oil production and increasing oil production. Along with the continuing research and exploitation of high-temperature reservoir, it becomes more important and deserved to do research on high-temperature resistant surfactants. According to the characteristics of high-temperature reservoir and its development status in China, high-temperature resistant surfactants was divided into anionic-nonionic surfactants, amphoteric surfactants, Gemini surfactants and fluorocarbon surfactants four types. What’s more, surfactants reviewed in this paper were also compared and it was found that some factors such as group and molecular structure can influence surfactant on its ability of temperature resistance. It was also pointed out that one of the most important direction of surfactant development is to do research on high-temperature resistant surfactant with the ability of biodegradation. At the same time, some suggestions about the synthesize of Gemini surfactant and the application of fluorocarbon surfactant were put off.
LUO Ming-liang , Si Xiaodong , Zhang Yu , Huang Wanli , Yang Zongmei , Gong Jincheng , Gong Jun
2018, 35(10).
Abstract:In view of poor film-forming stability and short-term protection of the conventional inhibitors in strong acidic medium, a microemulsion inhibitor(HSL-1)for coiled tubing was prepared by means of the liquid droplet and the quasi three-element-phase diagram method with employing dodecyl-trimethyl-ammonium bromide (DTAB), hexadecyl-trimethyl-ammonium bromide (CTAB), Mannich base, butanol and mineral oil as raw materials. The effects of HSL-1 mass fraction,acid mass fraction and environmental temperature on corrosion inhibition performance were investigated by using the static weight-loss method. The inhibition property and mechanism of HSL-1 for coiled tubing were also analyzed by virtue of the scanning electron microscope (SEM) and polarization electrical resistance measurement. The results showed that HSL-1 is a mixed type of inhibitor to inhibit the cathodic process and microemulsion with size of 15nm~85nm possesses an O/W structure; the inhibition of HLS-1 for coiled tubing under downhole condition is better in acidic medium when the HSL-1 mass fraction is in the range of 1.0~2.0 % and the corrosion rate is less than 3~5 g/ (m2·h). At the same time, the release rate of the active components can be controlled by the O/W structure of microemulsion and the effective mass fraction of inhibitor in the flow-back fluid was maintained, still keeping very low corrosion rate of 0.381 g/(m2·h) after the CT80 coupon immersed 12h in spent acid and the long-term inhibition for coiled tubing can be obtained.
LI Wei-yu , YI Zheng-ming , WANG Qing-yi , QIAN Jing-ru , DONG Yu-jie
2018, 35(10).
Abstract:Rosin-styrene acrylic composite emulsion was prepared by emulsion polymerization using styrene(St), methyl methacrylate(MMA), 2- ethylhexyl acrylate(2-EHA), 2-hydroxyethyl acrylate and acrylic acid as monomer. Using rosin emulsion as modifier made rosin styrene acrylic composite emulsion by emulsion polymerization. The effects of the amount of emulsifier, initiator, rosin emulsion and the ratio of monomer on the properties of emulsion were discussed. Then the composite emulsion was characterized by thermogravimetric analysis (TGA), dynamic light scattering particle size analysis (DLS), transmission electron microscopy (TEM). The results showed that the resulting emulsion with its particle size of 127 nm presented white with blue phase when the amount of the emulsifier, initiator ,rosin emulsion , hard and soft monomer ratio were 5wt%, 0.8wt% , 30wt% and 2.5:1,respectively. And more, the resulting film was absolutely smooth and transparent with good hardness, water resistance and adhesion properties.
2018, 35(10).
Abstract:A Hyperbranched polymer was synthesized from polycyclodextrin (HCD), acrylamide (AM), methacryloxyethylsulfobetaine (BTAM) as monomer by aqueous free radical polymerization via create-hydroxyl initiator system. The polymer possessed spherical nucleus and zwitterionic functional segments. The effects of polymerization time (T1), amount of the initiator dosage (M[O]), HCD dosage(MHCD), hydrolysis drying temperature (t) and BTAM dosage (MBTAM) on the polymer solution viscosity were investigated. The structure of the obtained polymer was characterized by 1HNMR and the solubility, thickening property, shear resistance, salt tolerance and anti-aging property were evaluated. The results indicated that the optimum polymerization conditions were T1=5.5h, M[O]=60mg, MHCD=20-30mg, t=120oC, MBTAM=200mg. In the 9374.13mg/L mineralized water, the basic dissolution time of HCD-HPAM-BTAM polymer was less than 40min, the viscosity of 2000mg/L polymer solution can reach 31.2 mPa?s, and the viscosity retention rate after shearing by the Waring stirrer level 1for 20s was as high as 80%, and viscosity retention rate after 90 days aging was as high as 63%, which were all better than the unmodified HPAM polymer.
Xiao Qiangqiang , Li Li , Ouyang Xinping , Yuan Wenhui
2018, 35(10).
Abstract:Aluminium nitride (AlN)/epoxy thermal conductive adhesive was prepared with epoxy as matrix material, AlN as thermal conductive filler. The structure and properties of adhesive were characterized using fourier transform infrared spectrometer, scanning electron microscopy, thermal gravimetric analyzer and thermal constants analyzer. The experimental results showed that coupling agent molecule was successfully chemically grafted onto the AlN surface. Modified AlN had strong interface adhesion with epoxy. The thermal stability and thermal conductivity of epoxy adhesive can be significantly improved by modified AlN. When the AlN mass fraction was 70%, the thermal conductivities of modified AlN/epoxy and AlN/epoxy adhesive were 2.24 W/(m.K) and 1.73 W/(m.K), respectively. In order to further improve thermal conductivity, hybrid filler of modified AlN and graphene oxide (GO) was employed to prepare thermal conductive adhesive. When the mass fractions of modified AlN and GO were 50% and 3%, the thermal conductivity of epoxy adhesive reached 3.05 W/(m.K).
SUN Li , Xu Li-yang , Li Hong-yang , Yang Ying
2018, 35(10).
Abstract:Abstract:To obtain electrode materials with high performance of supercapacitor, porous graphite carbon with high nitrogen level (NPGC) was prepared via a novel aggregation-NaOH activation route, in which low-cost kelp and melamine severed as carbon and nitrogen source, respectively. The as-prepared samples were characterized by XRD, BET, Raman and XPS. The results showed that the resulting NPGC with a lamellar structure displayed a large surface area of 1771 m2/g and a high graphite degree (ID/IG:2.84) and possessed a high nitrogen content of 6.27at%. In addition, the electrochemical properties of the samples were examined using cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS). As a result, the specific capacitance of the NPGC material reached up to 267 F/g at 1 A/g. Furthermore, the specific capacitance of the sample was still 99.9% of the initial specific capacitance after 5000 cycles. Thus, the synthesized material had excellent energy storage properties.
Wang Yuan , Zheng Hao , Ye Xiaofeng , Luo Yong
2018, 35(10).
Abstract:Salicylaldehyde imine ligand (1) and bis(phenoxy-imine) zirconium dichloride complex (2) have been synthesized. Both ligand and complex were characterized by mass spectrum, 1H NMR and 13C NMR. In the presence of MAO as a cocatalyst, the complex 2 was capable to catalyze ethylene polymerization. 2 displayed ethylene polymerization activity of 53.5 kg of PE/mmol of Zr.h at 50 oC and 0.9 MPa pressure in toluene, resulting in ultra-high molecular weight polyethylene with a viscosity average molecular weight value of 3.3x106 g/mol. The introduction of n-hexane as reaction solvent could further increase the molecular weight of obtained polymer to 4.1x106 g/mol.
2018, 35(10).
Abstract:The ploy-o-methoxyaniline composites (POMA-H-GA) was prepared by chemical oxidation polymerization with sulphuric acid and gallotannic acid as dopant and o-methoxyaniline as monomer. The structures of POMA-H-GA eigenstate were characterized by fourier transform infrared spectroscopy,X-ray diffraction,SEM and specific surface aperture analyzer. In addition, adsorption porperies of POMA-H-GA for Cr3 were investingated. The main factors of impacting Cr3 , initial concentration, time, adsorption temperature and pH were studied. The results show that the adsorption effect of the POMA-H-GA on adsorption of Cr3 achieves 467mg/g when the initial concentration of Cr3 is 12 mg/mL, time is 120 minutes, temperature is 20 degree and pH is 5 celsius, the order of adsorption amount of several metal ions is Cr3 Hg2 Pb2 Cd2 .
Wang Qiang , Wang Nai-wei , Fu Rui-feng , Jiang Zhidong
2018, 35(10).
Abstract:The Pd/SAPO-5 bifunctional catalysts were prepared by hydrothermal method, with triethylamine as the template, for one-step synthesis of methyl amyl ketone (MAK) from acetone and butyraldehyde. The influences of n(SiO2):n(Al2O3) and reaction temperature were investigated, and the properties of catalysts were characterized by H2-TPR, XRD, SEM, XRF and 29Si MAS NMR. It’s proved that while the doping of Pd didn’t change the molecular sieve crystalline structure of SAPO-5, the alteration of n(SiO2):n(Al2O3) could induce the changes in crystalline structure and morphology of SAPO-5. With the SAPO-5 crystalline structure kept intact, the activity of Pd/SAPO-5 rose with the n(SiO2):n(Al2O3). For the catalyst with the best n(SiO2):n(Al2O3) of 1.5 and operated at the optimized 180 ℃, the yield of MAK can be 58.2%, which is rather stable under 500h time-on-stream test.
JIN Dan , GUO Yu-peng , SUN Ke-wei , DING Dong-hai
2018, 35(10).
Abstract:The Graphene/Fe3O4/FeSiAl composite was prepared by hydrothermal method. Crystal phase, microstructure and wave absorbing property of the Graphene/Fe3O4/FeSiAl composite were characterized by XRD, Raman, SEM, FTIR and PNA. The results shown that graphene oxide was reduced to graphene by hydrothermal method. And FeSiAl magnetic flakes were coated by graphene and Fe3O4 particles evently. The absorbing material with both magnetic loss and dielectric loss can be realized by composite of flaky and granular. As the mass ratio of graphene oxide with FeSiAl increases, the effective absorption band (RL<-10 dB) of graphene/Fe3O4/FeSiAl composites is moved to higher frequency, which is positive for the application of the absorbent material in the high frequency band.
2018, 35(10).
Abstract:Loofah graft copolymers (loofah-g-PDMAEMA) was synthesized via electron transfer for atom transfer radical polynerization(ARGET ATRP), using loofah with bromide side-group(loofah-Br) as the macroinitiator and N,N,N′,N′,N″-pentamethyldiethylenetriamine (PMDETA)/copper(Ⅱ) bromide(CuBr2) as catalytic system, vitamin C as reducing agent. Chemical structure, crystalline structure and thermal stability of modified loofah were characterized by fourier transform infrared spectroscopy(FT-IR), thermogravimetric analysis(TGA). The lead adsorption and repeated adsorption performance of the loofah-g-PDMAEMA were studied. The results indicated that loofah-g-PDMAEMA possesses good adsorption capacity of Pb2+. loofah-g-PDMAEMA achieved the maximum adsorption capacity of 107.8mg/g under the best adsorption conditions when the temperature was 30°C, the pH was 5.5, and adsorption time was 5h. The adsorption process was conformed well to the pseudo-second-order kinetic model. Besides, after 5 reuses, the adsorption capacity can reach 84.73% of the first adsorption.
ZHANG Wen , WANG Xue-chuan , YU Ting-ting , LIU Yi-xiu , PENG Xiao-xue
2018, 35(10).
Abstract:Bacterial cellulose (BC)/ polylactic acid (PLA) composite film was prepared with PLA by A. Xylinum which could synthesize BC. Using the drug-loading rate as a indicator, the fermentation time, electrospinning speed and volume of PLA solution were studied to optimize the process of BC/PLA composite film. The chemical groups, thermal properties, mechanical properties, crystallinity and surface morphology of the BC/PLA composite film were analyzed by FTIR, TG, tensile test, XRD and SEM. The results indicated that the volume of PLA solution showed a small effect, and the optimal process was determined as follows: the electrospinning speed was 0.15 mm/s, the fermentation time was 36 h, the drug-loading rate of BC/PLA composite film could reach to 2.51 mg /g in the potassium diclofenate solution (15 mg/L). FTIR, TG, tensile test, XRD and SEM results showed that BC and PLA could be combined successfully, through which the thermal properties and mechanical properties of PLA could be improved, and the composite film had a three-dimensional porous net-work structure. The drug-releasing process of film conformed to the first-order release dynamics model.
LI Hongwei , LI Zeyu , YUN Hongfei , JI Dong , LI Guixian
2018, 35(10):0-0.
Abstract:Highly dispersed Ru-PEGx/NaY catalyst was prepared by impregnation-precipitation method using PEG(400) as the dispersant and (NH4)2CO3 as the precipitant. The samples were characterized by XRD, TEM, H2-TPR, ICP-AES and XPS. The results showed that the suitable PEG(7.5 mL) could trap the Ru3+ ions, and then increased the repulsion among Ru3+ ions, thereby impeding the agglomeration of Ru particles. The catalytic performance of the different samples was evaluated via p-nitrotoluene (PNT) liquid-phase hydrogenation to p-methyl-cyclohexylamine (PMC) reaction, with the PNT conversion and PMC selectivity as indicator. The results indicated that the catalytic performance of Ru-PEG7.5/NaY was the most excellent, the PNT conversion and the selectivity of PMC were found to be as high as 100 % and 95.0 % under the optimum conditions which the amount of Ru-PEGx/NaY catalyst was 0.50 g, reaction time was 35 min, the pressure of H2 was 3.5 MPa, the reaction temperature was 160 ℃, the amount of PNT was 5.00 g, stirring rate was 900 r/min and isopropyl alcohol was 300 mL. In addition, It was found that the activity of Ru-PEG7.5/NaY changed almost nothing after the fifth run, indicating the Ru-PEG7.5/NaY catalyst has good stability.
孙才英 , Jiang Dawei , Wang Ying , Huan Yinghong
2018, 35(10).
Abstract:Abstract: Atrovirens viscous liquid PAA/PANI-TiO2 was prepared by in-situ polymerization and ultrasonic oscillation method with 4, 4-two amino two phenyl ether (ODA) and pyromelliticdianhydride (PDMA) as the monomer, the PANI-TiO2 as the dopant, and then PI/PANI-TiO2 composite films were prepared by thermal imidization method. The structure, morphology and properties of the polyimide composite films were measured by means of FT-IR, SEM, TG-DTG, dielectric constant meter,and universal mechanical testing machine compared with PI film. The results showed that the thermal imidization of PI/PANI-TiO2 composite films was completely and the PANI-TiO2 particles were evenly distributed in the PI matrix. The tensile strength of PI/PANI-TiO2 composite films were increased from 14.8 MPa to 43.8 MPa with the addition of 10% mass fraction PANI-TiO2 particles, the initial degradation temperature was increased from 435℃ to 518℃ compared with pure PI, relative dielectric constant was increased from 3.38 to 3.86, dielectric loss factor was increased from 0.0013 to 0.0040. As a result the mechanical properties and thermal stability of PI/PANI-TiO2 composite films were enhanced compared with pure PI, the relative dielectric constant and dielectric loss factor were also increased.
GUO Xiaoyan , LIU Yuejiao , LIU Lixia , KONG Minfang , JIN Haibo , FAN Daidi
2018, 35(10).
Abstract:BaSO4 microspheres with a uniform diameter have been prepared in the presence of EDTA•2Na. The structures of BaSO4 microspheres were characterized by XRD, FTIR, XRF,SEM and particle size analyzer. The factors of EDTA•2Na dosage, the concentration of BaCl2 and Na2SO4, reaction temperature and pH adjusted once again were investigated. The prepared conditions are: c(BaCl2)=1.0 mol/L, n(EDTA•2Na):n(BaCl2):n(Na2SO4)=1:1:1,reaction temperature was 55 ℃ and pH was 9.0. Results showed that the particles are BaSO4. Monodisperse microspheres with the diameter ranging from 1.3 to 0.8 μm account for 47.01% of all particles. The yield of BaSO4 microspheres was 74.15%. When pH is adjusted once again to 7.0, the yield of BaSO4 increases from 74.15% to 87.88%. Meanwhile, BaSO4 diameter differs from sub-micron scale to 2 μm, which decreases the dimensional uniformity.
2018, 35(10).
Abstract:Self-assembledmonolayers (SAMs) of 2,5-Diphenyl-1,3,4-oxadiazole (PPD) synthesized by 2-ary1 hydrazine were fabricated on carbon-steel surface.The preparation conditions and corrosion inhibition of PPD SAMs were investigated by electrochemical measurement and surface analysis techniques. The inhibition mechanism of oxadiazole was further discussed by quantitative calculation. The results showed that the film assembled at4 mmol•L-1 concentration for 12 h possessed the best inhibition efficiency,which was up to 91.95%.The monolayers on the steel surface were detected through the X-ray photoelectron spectroscopy (XPS). The active region was verified by quantum chemistry calculation.
2018, 35(10).
Abstract:The photochromic microcapsule with narrow particle size distribution and smaller average particle size was prepared by emulsification-chemical crosslinking method utilizing spiropyran photochromic dye as core material and chitosan as shell material.The effects of emulsifier types, ultrasonic time and core-shell mass ratio on the particle size of microcapsule were investigated. The thermal stability and photochromic properties of photochromic chitosan microcapsule were studied. The results showed that the particle size distribution was narrow and the average particle size was 3.2 μm when the emulsifier was Tween80 and the mass fraction was 5% in the aqueous solution, the ultrasonic time was 2 h and the core-shell mass ratio was 1:3. The microcapsules prepared under these conditions were able to withstand the high temperature about 300 °C.The times of photochromic microcapsule dispersion to achieve color and fade steady state were 4.25 s and 26.00 s, respectively. The time of photochromic microcapsule dispersion to achieve color and fade steady state was only 0.25 s and 4.00 s higher than that of the photochromic dye dispersions. Moreover, the photochromic microcapsule had good photochromic reversibility.
FENG Jian-yan , Wang Xue-chuan
2018, 35(10).
Abstract:The epoxy modified grapheme oxide (EPGO) was synthesized via the epichlorohydrin (EPI) modified graphene oxide (GO). EPGO was characterized for its structure and morphology by FTIR, XRD and TEM.EPGO/WPU composites were prepared containing different mass fraction of EPGO (in the effective content of WPU), and the tensile and abrasion resistances of these films were tested. The results revealed that the addition of EPGO could increase WPU tensile strength obviously. When the addition amount of EPGO was 0.8wt%, composite materials tensile strength reached 12.9MPa. Compared with the blank film(without EPGO),tensile strength improved 67.5%,Young modulus enhance 39.2%, and the abrasion resistance of the film is improved obviously. So the mechanical properties of EPGO/WPU composites were strongly enhanced that is associated with the addition of EPGO.
2018, 35(10).
Abstract:A serious of hydroxyl silicone oil modified sulfonated waterborne polyurethane was synthesized with sulfonated polyester diols (BY3301), toluene diisocyanate (TDI) as the main raw materials, hydroxyl silicone oil as the modifier and with trimethylol propane(TMP) as the crosslinking agent. The structure and properties of the obtained polymer were characterized by FTIR and TG,digital display viscosity meter,nanoparticle size analyser, etc. And the effects of hydroxy silicone oil content on the properties of emulsion and film were investigated. The results show that with the increase of content of hydroxy silicone oil, the properties of polymer had been improved obviously.the particle size of the emulsion increases and the viscosity decreases, the water contact angle increases, and water absorption of film decreases. The tensile strength of the film gradually increases, and the elongation at break increases. When hydroxyl silicone oil content is 3%, the film has the best comprehensive performance. At the same time, the emulsion particle size is 85.1 nm, viscosity is 114.5 mPa•s, water contact angle is 91.7°, the tensile strength is 14.78MPa, the elongation at break is 427%, water absorption of 24 h is 5.61%. The TG curve shows that when the loss of film quality is 5%, the corresponding temperature is 269.9 ℃, increased by 17.3 ℃ compared with unmodified.
LIN Zhuang , Wang Rui , Gong Hong , Jiang Heng
2018, 35(10).
Abstract:Abstract:β-Cyclodextrin/epichlorohydrin copolymer(β-CDP) was synthesized in alkaline medium using β-cyclodextrin as monomer and epichlorohydrin as crosslinker. β-CDP was used as adsorbent for the adsorption of diphenolic acid (DPA) from the water solution. The influence of pH and β-CDP to DPA mass ratio for the DPA adsorption was investigated. The results showed that the adsorption efficiency was fairly good when the pH was less than 4.3 and the mass ratio of β-CDP to DPA was 12.5. At the same time, the mechanism of β-CDP adsorption for the DPA was discussed. β-CDP had a rapid adsorption rate for the removal of DPA from water solution, the hydrogen bond and hydrophobic interaction had important effort on the adsorption process. The adsorption kinetics agreed with the pseudo second-order kinetic model. Langmuir and Freundlich isotherm models were well described. The thermodynamic experiment was spontaneous and exothermic in nature. β-CDP had good regeneration performance, the adsorption capacity of β-CDP was 90% after five cycles of adsorption-desorption.
2018, 35(10).
Abstract:In order to study the effect of low-salinity water composition on the surface charge, wettability and oil film desorption capacity of rock and crude oil as well as the relationship between them. low-salinity water prepared by different ions in varied ionic concentrations and pH values were mixed with simulated rocks and crude oil samples to measure the Zeta potential value,respectively. The solid/brine water/crude oil three-phase contact angle was measured on the man-made core slices. The oil film desorption capacity on the surface of rock particles mixed with brine water was measured. The experiments showed that the effect of Na , Ca2 and Mg2 ions on the surface charge of crude oil and rock are mainly depended on the ionic valence state. The divalent ions have a more significant influence on the negative charge. The negative charge detected in solutions of the same ions decreases with the increase of the concentration of ions. The effect of increasing pH on negative charge is related to the ionic valence and the dehydration of solutions. The negative charge of the divalent Ca2 or Mg2 ion is less than that of the monovalent ion solution, and displayed a trend that the negative charge increased initially and then decreased,which differs from the latter . The results indicated that the effect of low-salinity water on the surface charge of crude oil and rock is consistent with the influence on the interfacial contact angle and the oil film desorption capacity. As the absolute value of the Zeta potential decreases, the interfacial contact angle increases and the oil film desorption decreases.
CHANG Dong-mei , QI He-dong , GUO Li-mei
2018, 35(10):0-0.
Abstract:Under aqueous solution polymerization method,acrylamide and sodium acrylate as polymerization monomers, bentonite as filler,polyethylene glycol diacrylate and N, N'-methylene bis acrylamide as crosslinking agents, potassium persulfate and sodium sulfite as initiators. The effects of various factors on the properties of temporary plugging agent were investigated by changing the bentonite, crosslinking agent, initiator dosage and the neutr-alization degree of acrylic acid . The results showed that when the reaction temperature was 50℃, the amount of crosslinking agent was 0.02% (the percentage of monomer mass,initiator), the amount of initiator was 0.6%, the amount of bentonite was 5% (the percentage of total mass),80% neutralization degree of acrylic acid. the temporary plugging agent,which synthetised by this way, its rate of the water absorption was 158 g.g-1 and its dissolution time was 21 hours at 80℃. Sulfonated asphalt were added to improve the degradation rate of temporary plugging agent, the polymer characteristic group was measured by Fourier transform infrared spectrometer, and the form of temporary plugging agent was characterized by SEM. And the effect was observed by reservoir core plugging experiment.
2018, 35(10).
Abstract:[(4-Dimethylaminophenyl)]di(tert-butyl)phosphine was prepared in two steps. Dichloro-4-(N,N-dimethylamino)phenylphosphane was firstly synthesized from N,N-dimethylaniline and PCl3 as starting materials. And the title compound was funished by coupling reaction of dichloro-4-(N,N-dimethylamino)phenylphosphane and tert-butylmagnesium chloride. Structure characterization of the intermediates was conducted by methods of 31PNMR、1HNMR and HRMS. The optimum reaction conditions were determined as follows: n (N,N-dimethylaniline) : n (PCl3) : n (pyridine) = 1 : 3 : 3,the reaction temperature and time was 110 ℃ and 24 h, the yield of Ⅰ was 85.3%. In the coupling step, n(Ⅰ): n (CuI) : n (LiBr) : n (t-BuMgCl) = 1 : 0.1 : 0.2 : 3,[(4-dimethylaminophenyl)]di(tert-butyl)phosphine was got in yield of 83.4% at 40 ℃ for 12 h.
Bu Xin , PEI Ji-cheng , CHAN Hui-fang , ZHANG Fang-dong , LIU Hai-tang , ZHOU Zhi-min , ZHEN Xiao-qin , Wang Jing
2018, 35(10):0-0.
Abstract:Carboxylated-chitooligomer (C-COS), which had a high moisture-absorption and moisture-retention ability, was prepared by oxidation of chitooligomer using a laccase/ 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO) system. The intermolecular hydrogen bonding of C-COS was investigated by low-field nuclear magnetic resonance (LF-NMR), FTIR and 13CNMR, and its moisture-absorption and moisture-retention mechanism was deduced. The results showed that intermolecular hydrogen bonding were formed between polymer molecules and water in the course of C-COS hygroscopic process. More polar carboxylate ions on the C-COS molecule produced new hydrogen bonding effect. The decrease of the absorption peak intensity at 3363 and 1643 cm-1 and blue shift of the absorption frequency at the same wave number in the heating IR, as well as the increase of the absorption peak at 1643 cm-1 in the swelling IR, confirming that information of hydrated hydrogen bonds (H-O-H•••O-C=O) between water and carboxylate ions on the C-COS molecule. In addition, moisture-retention mechanism of C-COS was obtained that the polymer dissolved in the water system can form a huge polymer-water network structure, prompting the water molecule in the form of hydrogen bonds was firmly locked in this network structure.
Wang Linhan , Qaio Kaina , Ding Qi , Zhang Yuyu , Sun Baoguo , Chen Haitao , Sun Ying
2018, 35(10).
Abstract:In order to compare the effects of different cooking time on taste compounds in chicken soup, the chicken breast was taken as the object of study. Chicken soup samples were prepared by different cooking time. The contents of organic acids, 5’- nucleotides, free amino acids and taste peptides in the samples were analyzed by HPLC and amino acid automatic analyzer. The results showed that the pH value of chicken soup decreased at first and then increased with the heating time, reaching a minimum of 6.39 at 3 h; The contents of CMP, GMP, lactic acid and amino acids in chicken soup increased gradually at 1-5 h, and the content of 5’- nucleotides IMP and AMP reached the maximum of 14.22 ?g/mL at 2 h and of 48.72 ?g/mL at 3 h, respectively, the content of succinic acid was always 0.39 mg / mL after 2 h, and the content of glutamic acid reached the maximum value of 291.39 μg / mL at 5 h, which had great contribution to chicken soup flavor. The EUC value of chicken soup increased with the cooking time and reached the highest value of 0.28 at 5 h. The content of umami peptide increased with the increase of heating time, and reached the maximum value at 4 h, which was 12.06 mg/mL, indicating the maximum flavor. The content of umami peptide increased with the increase of heating time, and reached the maximum value at 4 h, which was 12.06 mg/mL. Sensory analysis showed that at 2-4 h, the chicken flavor was significantly increased and then weakened.
KUANG Xinmou , Sun Yin , WU Zhi-ge , He Xirui , CHEN Xu-fei , BAI Ya-jun
2018, 35(10):0-0.
Abstract:In this paper, L-valine and menthol was used as raw materials,then valine menthyl eater was synthesized with DCC / DMAP as catalyst, The structure of the compound was identified by MS, MR and IR.Then, bioactivity of anti-epilepsy and antitumor were carefully measured by the method of maximal electrical shock convulsion experiment(MES)and Inhibition of HeLa cell growth experiment respectively。it showed that:(1) In the maximal electrical shock convulsion experiment, mice were injected intraperitoneally, when valine melaminate was dosed at 100 mg / kg, compared with saline and carbamazepine groups, four experimental mice, The convulsions number of mice after 0.5, 1, 2, 3 and 4 h were 2, 2, 2, 1 and 0, respectively, which showing antiepileptic activity similar to the reference substance carboplatin ;(2) In the antitumor experiments, growth of HeLa cells were significantly inhibited,and the highest inhibition rate reached 52.5%.
2018, 35(10):0-0.
Abstract:In order to obtain blend hydrogel system which has better performance and is more suitable for applying in food industry, rheological properties of Tara Gum/Konjac Glucomannan (TG/KGM) gel system in different proportion were studied by rotational rheometer in this research, the interaction between KGM molecular chain and TG molecular chain was studied by means of statistical mechanics and dynamics as well. Result reveals that TG/KGM gel behaved like pseudoplastic fluid at high temperature and the two polymers had good compatibility. The shear stress, viscosity and shear resistance all increased with the increase of the proportion of KGM. In the selected frequency range 0.1~100 rad/s, the loss modulus G”of TG/KGM is lower than storage modulus G ', and the addition of KGM caused both modulus rised. However, during the cooling process of 85~25℃, G 'and G' modulus decreased with the increase of the proportion of KGM, and the conversion temperature of sol to gel gradually increased, Thus, it is showed that compared with the single polysaccharide, the proper proportion of TG/KGM could greatly improve the heat resistance and form the gel with higher stability. Especially when m(TG):m(KGM)=0.9:0.6 (TK6), a gel system with more excellent comprehensive properties, higher gelling ability, higher stability and more moderate viscosity can be obtained. This kind of TG/KGM gel is expected to become a new type of gel applying in food industry, which can provide theoretical guidance for the rational application of TG and KGM.