ZHU Zi-pei , ZHONG Lian-jun , HE Qi , XIAO Kai-jun
2017, 34(6).
Abstract:In order to improve the anti-fouling property of PES membrane, the PES was first sulfonated, by using the interaction between the sulfonated groups and silver ions. Then, the nanosilvers were introduced onto the surface of sulfonated polyethersulfone (SPES) membranes by using vitamin C as reducing agent to fabricate the sulfonated polyethersulfone membranes with nanosilvers (SPES@Ag). Characterization of the SPES@Ag membrane was carried out by scanning electron microscopy(SEM), atomic force microscope(AFM) and X-ray diffraction(XRD), antibacterial performance was studied by viable cell attachment test as well. It is show that nanosilvers were successfully loaded onto the surface of SPES and the size of nanosilvers is about 120 nm. The SPES@Ag membrane showed excellent anti- fouling property. The antibacterial rate reached 96.7%,98.3%,87.7% for E.coli, P.aeruginosa and S.aureus respectively, The results of the flux and rejection tests are shown that fiux was 438.4 L/m2.h and the rejection of BSA reached 94.5%.
2017, 34(6).
Abstract:Hierarchical structured SAPO-5 molecular sieve has been ionothermally synthesized by microwave irradiation and using eutectic mixture based on succinic acid/partly succinic acid with sebacic acid, choline chloride and tetraethyl ammonium bromide as solvent and template.The influences of various experimental parameters, such as crystallization time, the types of precursors and the kinds of eutectic mixture have been systematically investigated. The resulting SAPO-5 molecular sieve was characterized by X-ray diffraction (XRD), Scanning electron microscope (SEM), and N2 physical adsorption-desorption, respectively. SEM analysis revealed that aluminum and phosphorus sources had great impact on SAPO-5. N2 physisorption measurements confirmed that replacing partly succinic acid with sebacic acid has great impact on the pole structure of SAPO-5. SEM、N2 physical adsorption-desorption characterizations show that the resultant material is one kind of hierarchical structured aluminophosphate molecular sieve possesses both micropore and mesopore.
WANG Yan-lin , HE Jing , YANG Hai-jun
2017, 34(6).
Abstract:A caged phosphorothioate flame retardant synergistic with silicon, phosphorus and sulfur three elements, diphenyl silicic acid bis-1-phosphorus heteroaryl thio-2,6,7-trimethyl- oxabicyclo [2.2.2] octyl-4-methyl ester, was synthesized by dimethoxydiphenylsilane (DMDPS) and 1- phosphorus heteroaryl thio-4-hydroxymethyl-yl-2,6,7-trimethyl- oxabicyclo [2.2.2] octane (SPEPA).The effects of solvent, reaction temperature, reaction time and mass ratio on the yield were investigated. The optimal conditions were selected as follows: n(DMDPS): n(SPEPA) is 1:2.2, kept the reaction going at 140℃ , then fractionating for 7h and the yield can reach to 92.7%.The structure and flame retardance of the product were characterized by means of FTIR, 1H -NMR, TG-DTA analysis and LOI technique. Results showed that the product have a good thermal stability and high flame-retardant and anti-dripping efficiency for polybutylece terephthalate (PBT). Besides, when it was mixed with MPP and was applied to PBT, high synergistic flame-retardance efficiency was found.
ZUO Fang , Du Sinan , Luo Yang , Li Xinhua , Liu Dong
2017, 34(6).
Abstract:Magnetic Fe3O4 nanoparticles (NPs) were prepared by coprecipitation method. The Fe3O4@PDA nanoparticles (PDA@Fe3O4 NPs) were synthesized by in-situ polymerization of dopamine (DA) on Fe3O4 NPs surface, and then utilized as heterogeneous Fenton catalysts for degradation of methylene blue (MB). The morphology, structure and composition of the samples prepared were characterized by transmission electron microscope (TEM), X-ray diffraction (XRD), Fourier-transform infrared (FTIR) spectra and X-ray photoelectron spectroscopy (XPS). Moreover, the catalytic activity and stability of the Fe3O4@PDA NPs were investigated and the possible catalytic mechanism was also discussed. The conditions were 0.6 M of H2O2 concentration,1.16 mg/L of catalyst dosage, 7.0 of pH and 25 mg/L MB mass concentration. Under the above conditions,the degradation efficiency of MB were only 26% in case of Fe3O4 NPs as catalyst within 2 h, while Fe3O4@PDA NPs exhibit higher catalytic activity with 99% MB degradation efficiency after 30 min. The results suggest that the existence of PDA which has phenol and qunione units in Fe3O4@PDA NPs promoted the cycle of Fe3+ to Fe2+, which induced the higher catalytic activity compared with Fe3O4 NPs. Moreover, Fe3O4@PDA NPs, with an excellent stability, could be reused three times and continue to the cycle reaction after regeneration by reaction with NaBH4.
2017, 34(6).
Abstract:Raw materials that nanometer V2O5, nanometer Cr2O3 and nanometer carbon were calcinated in N2 atmosphere after dried and mixed by high energy milling, then VN/CrN nanocomposite were synthesized. The products were characterized by XRD、TG-DSC、SEM、BET and TEM. The results show that VN/CrN nanocomposite with an average crystallitesize of 40 nm can be synthesized at 1200 ℃ for 2 h. The as-prepared nanocomposite is mainly composed of VN, CrN and VCrN2. These 3 constituents are all face center cubic crystals and belong to space group Fm3m. Different weight percent of nanocomposite was used as additive and was added to the vitrified bond. The test result shows that when w (composite)=0.2%, the bending strength and liquidity could be increased by 20% and 50%, respectively. When w (composite)=1.0%, the bending strength and liquidity reach the maximum, which are 115.6 MPa and 207.2% , respectively.
2017, 34(6):0-0.
Abstract:A series of ZnO, Al-ZnO and x-Mn-Al-ZnO adsorbents were synthesized by co-precipitation methods and investigated for the H2S desulfurization at ambient temperature.Thedifferencecaused by Mndopants in terms of structural properties, crystal structure, morphology and chemical state of reactive sites, were systematically investigated by N2adsorption, X-ray diffraction (XRD),scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), respectively. The results show that with the increasing of Mn dopants, the desulfurization performance has two extreme points, when doping 0.02 mol and 0.08 molMn to Al-ZnO matrix. According to the characterization and desulfurization performance, different amount of Mn dopants leads to different promotion mechanism. The great performance of 0.02Mn-Al-ZnO is attributed to large surface area of 171.4 m2/g. Despite the surface area drops along with the increasing doping of Mn, more Mn enter into ZnO crystal lattice,which enhances the interaction between Zn and Mn, resulting in a promotion ofdesulfurization performance.However, the further doping ofMn results in smaller surface area and formation of ZnMn2O4, which causes poor desulfurization performance.And the highestsulfur capacity can be obtained over 0.08 Mn-Al-ZnO with 7.21g S/100 g sorbent, under 25oC, GHSV of 3000 h-1and 1000 ppmv H2S. It reveals clearly that doping difference amount of Mn can change morphology, crystal structure and physicochemical properties in varyingdegree, and each of them can act as a major factor leading to various desulfurization performance.
2017, 34(6):0-0.
Abstract:Olivine structure of lithium iron phosphate (LiFePO4) has been recognized to be the most promising cathode material for electric vehicle due to its high theoretical capacity, outstanding thermal stability, and excellent cycling stability. Nano/micro porous structure LiFePO4/C composites were synthesized by wet milling-spray drying-carbothermal reduction method. X-ray diffraction (XRD), scanning electron microscopy (SEM), were used to determination the morphological structure of materials, constant current charge-discharge test is used to determination the effects of calcination conditions on the electrochemical performances of LiFePO4/C. The results show that: sintered at 650 ℃ for 8.5 h, the sample delivered a discharge capability of 123 mAh?g-1 with no capacity loss after 100 cycles at 10 C under room temperature, showing better discharge capability and cycle performance, these advantages were useful for the application of power batteries.
2017, 34(6):0-0.
Abstract:A terpolymer ESA/IA/SS was synthesized by copolymerization using epoxysuccinic acid (ESA), itaconic acid (IA) and sodium p-styrenesulfonate (SS) as monomers and ammonium persulfate as initiator. The structure of product was determined by IR. In addition, the effects of mass radio of MA and IA, initiator amount, reaction temperature and reaction time on the properties of the polymer. And The optimal synthesis conditions was obtained. when the m(MA):m(IA)=3:1, the amount of SS and initiator accounted for 20% and 12% of the total monomers mass respectively, the reaction temperature was 85 oC and the reaction time was 4 h, the viscosity average molecular weight of the product was 1176.3. The properties of scale inhibition and dispersion of ESA/IA/SS were studied and compared with those of ESA/SS and PESA. The results showed that the property of inhibition to CaCO3 scale of ESA/IA/SS was similar to that of PESA. When the dosage was 50 mg/L, the scale inhibition rate of PESA was 72.3%, and that of ESA/IA/SS was 71.5%, which was 27.3% higher than that of ESA/SS. For the property of inhibition Ca3(PO4)2 scale, ESA/IA/SS was much higher than PESA. When the dosage was 40 mg/L, the rate of scale inhibition of PESA was only 7.0%, while that of ESA/IA/SS was 98.6%. Beside, ESA/IA/SS had a certain property of dispersing Fe2O3, the light transmittance of the FeCl3 solution with ESA/IA/SS kept at 72.6%.
LU Xiang , HE Zheng-yi , LEI You-xin , QIN Zhi-yong , LIU Zu-guang
2017, 34(6).
Abstract:Abstract: A novel surfactant was prepared from lignin-amine modified by rosin ester, which was synthesized from rosin and epichlorohydrin. The surfactant was characterized by IR 、UV and the automatic surface tensiometer, and its physico-chemical properties were also measured. The introduction of abietyl groups as hydrophobic groups in lignin-amine, by O-alkylation reaction, enhanced the performance of the surfactant. The experiment results showed that the synthesis conditions for rosin ester were optimized as follows: the molar ratio of rosin to epichlorohydrin was 1: 1.5, reaction temperature was 100℃, reaction time was 6h. Under these conditions, the conversion rate of rosin was up to 95.6%. When the molar ratio of lignin-amine to rosin ester was 4, the surface tension of the surfactant reached 33.2 mN/m at a concentration of 10 g/L hydrochloric acid aqueous solution with a pH 2.0. The emulsifiability of the surfactant was 74 min. In contrast, the surface tension of lignin-amine at the same condition was 48.5 mN/m, and it’s emulsifiability was 43 min. As expected, the performance of the surfactant was improved by abietyl groups.
WANG Peng-fei , ZHA Fei , CHANG Yue
2017, 34(6):0-0.
Abstract:Load-type methanol dehydration catalyst of (SAPO-34)-kaolin was prepared by hydrothermal method using kaolin as a low-cost material and triethylamine as template agent. The synthesized catalysts were characterized by XRD, SEM, EDS, BET, H2-TPR and NH3-TPD techniques. The results show the synthesized SAPO-34 molecular sieves prepared by Si and Al of kaolin grow in situ at the surface of residual kaolin. (SAPO-34)-kaolin has good dispersity and relatively high crystallinity. CuO-ZnO/(SAPO-34)-kaolin was prepared through loaded CuO-ZnO to the surface of (SAPO-34)-kaolin, which can be used for synthesis of light olefins from CO2 hydrogenation. Under the condition of temperature at 673 K, pressure at 3 MPa, airspeed at 1800 mL/(gcath) and V(CO2) / V(H2) = 1:3, the one-way conversion of CO2 could reach up to 43.5%, with a light olefins selectivity and yield of 63.8% and 27.8%, respectively. For a continuous performance as long as 8 h, the yield of light olefins is over 18.7%.
WANG De-ju , LIU Zhong-neng , YANG Wei-min
2017, 34(6):0-0.
Abstract:Binderless mordenite zeolite with small crystal size of 100~200nm in c-axis direction was successfully prepared by a hydrothermal transformation method. The pre-formed precursor of aluminosilicate embedded with mordenite zeolite crystal seeds was converted into binderless mordenite zeolite with regular macro-morphology, high crystallinity and excellent mechanical stability. The catalyst for amination of ethanolamine to prepare ethylenediamine was developed based on the as-prepared binderless mordenite zeolite. The as-prepared catalyst exhibited good catalytic activity and selectivity for ethylenediamine due to high surface acidity and abundant porosity. At the reaction temperature 330~340 ℃, ethanolamine LHSV 0.40 h-1, n (NH3): n (MEA) =30, reaction pressure 1.8MPa, the catalyst stability test indicated that single pass conversion of MEA is about 50% and EDA selectivity is more than 70%, the total yield of EDA and PIP is about 40%. The catalyst remained stable for 1400 hours at the optimum reaction conditions. The activity of the catalyst recovered well after regeneration.
LIU Hong-liang , Jiang Ping-ping
2017, 34(6).
Abstract:Bismuth oleate(BO) was synthesized from acetic anhydride, bismuth oxide and oleic acid by two - step reaction, and it was added to polyvinyl chloride (PVC) as thermal stabilizer in order to improve its thermal stability. The structure of bismuth oleate was characterized by Fourier transform infrared spectroscopy (FITR), mass spectrum(MS) and the composition of bismuth oleate was determinated by elemental analysis(EA) and EDTA complexometric titrati. At the same time, the interaction mechanism of bismuth oleate improving the thermal stability of PVC was investigated by thermal aging oven test, Congo red test, conductivity test, thermogravimetric analysis (TGA) and rheological curve. The results showed that the time of the initial whiteness of PVC sheet with 2.6% bismuth oleate was 60 min, and the static stability time of Congo red was 39.5 min, so the thermal stability of PVC was improved obviously. The bismuth oleate could be used as a liquid thermal stabilizer. Moreover, from the analysis of the test of the bismuth oleate for HCl and complexing mechanism, we considered that the bismuth oleate could improve the thermal stability of PVC products mainly by the means of oleate ions substituting unstable chlorine atoms.
2017, 34(6).
Abstract:A novel thermal sensitive catalyst was synthesized by the reflux method and then added into the low density polyethylene (LDPE) film, the thermocatalytic degradation of films was conducted in oven with near room temperature under darkness. The obtained samples were characterized with Scan electron microscope (SEM), Energy dispersive analysis of X-ray (EDX), Mechanical properties, Atomic force microscope (AFM), Thermogravimetry (TG), Gel permeation chromatography (GPC) and Fourier transform infrared spectroscopy (FT-IR). Results showed that the composite film was thermally degraded obviously, while pure polyethylene film changed slightly. After thermodegradation for 45 days under 55oC, mechanical properties decreased obviously of composite film, roughness increased significantly and some fold and scaly structure appeared on the surface, thermal decomposition temperature of which reduced by 13oC, molecular weight also significantly dropped, besides, the characteristic absorption peaks such as carboxylic acid and hydroxy were observed as well.
2017, 34(6):0-0.
Abstract:Copolymer AM/C5 was synthesized by copolymerization of hydrophobic monomer(C5 petroleum resin) with acrylamide, and then the novel hydrophobic polymer Mannich base was prepared from aminomethylation with copolymer. Effect of mass ratio of C5 petroleum resin and acrylamide, initiator dosage, reaction temperature and pH value on polymerization were investigated. Effect of reaction time, temperature and pH value on apparent viscosity of mannich base were discussed. The structure of products was characterized by FTIR and 1HNMR, and the performance analyzed. The results showed that the optimum conditions of copolymerization were as follows:reaction temperature 40℃, pH 8, initiator mass fraction 0.5% of the monomer mass, m(AM):m(C5)=15:1. The Mannich base solution has a higher value of apparent viscosity is 418 mPa·s under the conditions of reaction time 5 h, temperature 60~70℃, pH 9, n(AM):n(HCHO):n(NH(CH3)2)=1:1.1:1.5. When the temperature was 90℃, the viscosity reserved rate was more than 43.3%; when the mass concentration of NaCl、CaCl2 was 2000 mg/L, the viscosity retention rate was 32.8% and 21.7%,respectively. Therefore, the Mannich base possessed the excellent tackability; temperature tolerance and salt resistance.
2017, 34(6).
Abstract:Hydroxyl-terminated waterborne polyurethane (WPU) emulsions with different R values(-NCO/-OH) were synthesized firstly via acetone method, in which isophorone diisocyanate and poly (ε-caprolactone) di-OH are the main raw materials, with dihydroxy methyl butyric acid as hydrophilic monomer, triethylamine, 1, 4-butanediol, trimethylolpropane and organic silicon crosslinker as neutralizing agent, small molecule chain extender, inner-crosslinking agent and outer-crosslinking agent respectively. Then, two-component hydroxyl-terminated WPU adhesives with excellent properties were prepared by adding the 2% enclosed water-based isocyanate curing agents. The chemical structure, morphology and rheological properties of the adhesives were characterized by infrared spectroscopy, nuclear magnetic resonance, laser particle size analyzer, transmission electron microscopy and rheometer, seperately. Furthermore, the thermal and mechanical properties of the film were characterized via thermo-gravimetric analyzer and universal tensile testing machine. The results showed that comprehensive properties of adhesive prepared were best when R value is 0.85, the water absorption, tensile strength, elongation at break and peel strength of film is 19%, 14.74 Mpa, 236.53% and 0.421 KN/m, respectively.
kejiexi , Yang Feng , Wang Feng , Kang Maoqing , Wang Junwei
2017, 34(6).
Abstract:The main factors which had significant effects on the synthesis of carbonated polypropylene glycol diglycidyl ether (5CC-PPGDGE) were investigated by using uniform design. The 5CC-PPGDGE was synthesized from polypropylene glycol diglycidyl ether (PPGDGE) and CO2 by using quaternary ammonium salt modified amberlyst D296 as catalyst. Effect of D296 catalyst content, reaction time, reaction temperature, reaction pressure and catalyst activation time on conversion efficiency of PPGDGE were investigated. By two uniform design experiments, the main factors for PPGDGE conversion were determined: catalyst content = 12 %, reaction time = 38 h, reaction temperature = 125 ℃, reaction pressure= 1 MPa and catalyst activation time = 24 h, and the optimum conditions were obtained based on the relationship between experimental factors and conversion which was acquired through regression. The conversion of product from the optimum condition was almost 100 % and product was confirmed by FTIR, 1HNMR, 13CNMR, GPC and TGA analysis.
2017, 34(6).
Abstract:To study the influence of polyampholyte’s molecular structure on its rheology, the copolymers of acrylamide (AM) and diallyl dimethyl ammonium chloride (DMDAAC) were synthesized via free radical copolymerization, and then were hydrolyzed with NaOH to produce nine polyampholyte-hydrolyzed poly(AM/DMDAAC) (abbreviated by HPAD-1, HPAD-2, HPAD-3, HPAD-4, HPAD-5, HPAD-6, HPAD-7, HPAD-8 and HPAD-9) with varied intrinsic viscosity, anionicity and cationicity. These polymers were characterized by IR, 1H NMR, titration and Ubbelohde capillary viscometer. The apparent viscosity and shear thinning behavior of HPAD solution were studied by using rotational viscometer and rheometer, respectively. The results revealed that HPAD’s intrinsic viscosity was in a positive correlation with both its solution viscosity and shear thinning effect. The apparent viscosity of 0.75% HPAD solution (mass fraction) increased from 12.1 mPa•s (HPAD-9) to 766.5 mPa•s (HPAD-7) when the intrinsic viscosity grew from 182.03 mL/g to 555.08 mL/g. The anionicity and cationicity of HPAD were negatively correlated with solution viscosity, and had little influence on shear thinning behavior. The apparent viscosity of 0.2% HPAD solution (mass fraction) decreased from 111.1 mPa•s (HPAD-1) to 21.5 mPa•s (HPAD-4) when the anionicity enhanced from 29.98 mol% to 51.75 mol%. HPAD-2 and HPAD-8 with cationicity of 10.31 mol% and 6.88 mol% respectively, had almost coincided shear thinning curves in the range of 5 s-1 to 100 s-1.