2014, 31(5).
Abstract:The composite superabsorbent (CSA) with biodegradability was synthesized by using cassava starch mechanically activated for 60 min, acrylic acid and bentonite (BT) to enhance its water absorbency (Aeq) and retention. The effect of bentonite’s dosage on the water absorbency and the swelling properties of CSA were studied. The morphology, thermostability and functional groups of the samples were characterized by SEM, TGA and FTIR, respectively. The results showed that CSA had a microporous and laminate structure, the Aeq of CSA was increased from 1604 g/g to 1807 g/g by introducing an appropriate amount of BT (30 % to the weight of starch), and the thermostability and capacity of water-holding were also strengthened. The weight loss of CSA was 79.3 % when it was heated to 700 ℃, which was lower than that of superabsorbent without BT (83.4 %). The water retention for CSA was 48.3 % in the pressure of 1912 Pa and higher than that of superabsorbent without BT (45.5 %). Meanwhile, the swelling processes of CSA exhibited first-order dynamics, and the Aeq was of pH and salt dependent.
ZHAO Chen-xu , ZUO Fang , PAN Li , WANG Xiao-dan , LIAO Zhi-jian , QIN Zhen-li
2014, 31(5).
Abstract:Polydopamine (PDA) functionalized silver nanoparticles (PDA-nanoAg) were synthesized by one-step method with PDA as the reductant and protectant. The mechanism for preparation of PDA-nanoAg was proposed. The stable dispersion duration of the as-synthesized Ag nanoparticles in water was also observed. The structure and morphology of PDA-nanoAg particles were investigated by ultraviolet-visible (UV-Vis) absorption spectroscopy, transmission electron microscopy (TEM), and Fourier-transform infrared (FTIR) spectrometry. The antibacterial activity of PDA-nanoAg nanoparticles against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) were investigated by broth dilution. The results indicated that the average diameter of the Ag nanoparticles was 50 nm, and PDA-nanoAg particles exhibited good stability in water over a long period of time. The minimal inhibitory concentration (MIC) and the minimal bactericidal concentration (MBC) of the as-synthesized Ag nanoparticles against E. coli and S. aureus were 7.56 mg/L and 30.24 mg/L, respectively.
2014, 31(5).
Abstract:THEIC three silicate chloride ethyl was synthesized by using tri (2-hydroxyethyl) isocyanurate (THEIC),silicon tetrachloride and ethylene oxide as raw materials.The effects of solvent, reaction temperature and amount ratio of substance on product yield was discussed.The optimal conditions were selected as follows:n(silicon tetrachloride)﹕n(ethylene oxide)﹕n(THEIC)﹕n(ethylene oxide) was 3﹕6﹕1﹕3.3;Silicon tetrachloride was first reacted with ethylene oxide for 1h at 25℃,and then THEIC was added at 80℃ reaction for 8h,finally ethylene oxide was added at 40℃ reaction for 3h;The product was purified and the yield of product was 94.3%.The structure and properties of products was characterized by using FTIR,1H-NMR,DTA and limiting oxygen index techniques;The application experiments showed that the product contained silicon,nitrogen,chlorine three flame elements and had a good synergistic flame retardant synergism,it can be applied to polyvinyl chloride, polyurethane,epoxy resin and unsaturated resin polymer materials.
2014, 31(5).
Abstract:In aqueous buffer system containing surfactants (cetyltrimethyl ammonium bromide or sodium dodecyl sulfate or nonylphenol polyoxyethylene ether), the enantioselective reduction of 4’-chloroacetophenone to its corresponding chiral alcohol (S)-1-4’-chlorophenyl ethanol catalyzed by yeast cells were investigated. The results indicated that the conversion of 4’-chloroacetophenone was distinctly improved and the enantiomeric excess of product (S)-1-4’-chlorophenyl ethanol was barely changed when the surfactants were added to the system. Nonylphenol polyoxyethylene ether (NP-4) was the most appropriate additive among being added surfactants. In addition, the influence of nonionic surfactant NP-4 on the enantioselective reduction of aromatic ketones was studied. The results showed that the enantiomeric excesses of products (S)-1-aryl ethanol had little change and the conversions of all aromatic ketones were significantly enhanced in the presence of NP-4. It was also found that the increase of the substrate conversion was relevant to the electronic effect of the substituents on the aromatic ring. The stronger electron-donating capacity of the substituents was more beneficial to the increase of the substrate conversion.
WEI Si-bao , LI Jia-cheng , LIU Yan-feng , ZHANG Shi-xin , LI Ke , HUANG Jun-hao , LIN Qiang
2014, 31(5).
Abstract:The stable Pickering emulsions were prepared by SiO2 nanoparticles whose surface were combiningd with octyl-grafted amphiphilic alginate derivative(OAAD) hydrophobically modified by 1-Octyl amine. And the properties of OAAD, aqueous dispersion of OAAD/SiO2 nanoparticles and Pickering emulsions were characterized by means of Fourier transform infrared spectroscopy (FTIR),1H nuclear magnetic resonance(1H NMR),Surface tensiometer,fluorescence spectrum,dynamic light scattering,Contact Angle Meter and optical microscope studies. Experimental results showed that Octyl amine groups had successfully grafted to the alginate(SA) molecular chains. The surface tension of modified alginate was lower than SA and the critical aggregation mass concentration was reduced to 0.60g /L,which showed good amphipathy.When the water dispersion system was formed by adsorption of OAAD on the surface of SiO2 nanoparticles and used to prepare stable Pickering emulsions, it was observed that with the increase of OAAD’s mass concentration, the wettability of SiO2 nanoparticles increased, the zeta potential decreased and the particle size increased whereas the particle size of Pickering emulsions decreased that enhance the stability of Pickering emulsions. preliminary analysis of the mechanism, it was indicated that a certain concentration of OAAD adsorbed on the surface of SiO2 nanoparticles could lead to the flocculation among the inter particles, so that the network structure of interfacial film formed in the oil-water interface which was helpful to improve the stability of Pickering emulsions.
FENG Ying-ying , LIU Jun-zhong , ZHANG Hong-juan , LIU Qian , JIAO Qing-cai
2014, 31(5).
Abstract:Multi enzyme coupled catalysis is one of the important methods in the enzymatic preparation of chiral drug intermediates. In this study, the ammonia of L-aspartic acid was transferred to the phenylpyruvic acid, and L-phenylalanine with byproduct pyruvic acid were synthesized by aspartate aminotransferase (AspAT) whole cell. Then, L-tyrosine was enzymatic synthesized when substrate phenol and tyrosine phenol-lyase (TPL) whole cell were added into the reaction system. Some factors affecting dual enzymatic catalysis were investigated. The optimal conditions were 40oC, pH 8.5, 25 g/L of phenylpyruvic acid (PPA), n (PPA): n (L-Asp)=1:1.2, m (AspAT): m (TPL)=1:1, 4 mmol/L of PLP, 0.1 g/L of Tween 80. 30 g/L of ammonium chloride had a promoting effect on dual enzyme coupled catalysis reaction. The method biological synthesis of L-tyrosine with coupled dual enzyme in dual host, not only makes full use of the by-product of the reaction pyruvic acid for higher value-added products, but has reference significance for the reasonable utilization of resources and green synthesis process.
ZHANG Yang , WANG Dun , SUN Zhong-liang , CAO Xian-ying , CAO Yang
2014, 31(5).
Abstract:A Novel solid acid catalyst had been prepared from aromatic microporous organic polymers through a controlled sulfonation procedure. The sulfonated catalysts were characterized by FT-IR spectroscopy, X-ray diffraction, surface acidity, elemental analysis and BET method. Catalytic performance was determined via esterification of oleic acid with methanol. The results showed that the solid catalysts had high BET surface area (540 m2/g), pore volume (0.40 cm3/g) and the surface acidity was up to 2.9 mmol/g. The solid acids exhibited higher activity than amberlyst-15 for esterification of oleic acid, which conversion could reach 93% at 75℃ for 6h. The solid acid catalysts showed excellent regenerated properties.
2014, 31(5).
Abstract:Commercial beta molecular sieve as part of the silicon aluminum source, TEOS as silicon source and P123 as the template agent is the preparation of composite molecular sieves beta/SBA - 15 by adopting after synthesis under hydrothermal conditions. Investigating synthesis conditions,including acid concentration, acid volume, crystallization temperature and time and so on have the impact on the synthetic samples, and their structures were characterized by adopting XRD, FT-IR and N2 adsorption - desorption methods, the results show that the acid concentration is 6 mol/L, 40 ml acid volume, beta load 50%, the crystallization temperature of 110 ℃ and 48 h crystallization time is the best synthesis condition, beta secondary structural unit into the SBA - 15 hole in the wall, hole wall become thickening. Then comparing the catalytic effect of phenol alkylating of beta, mechanical mixing and synthetic samples clearly indicates that the sample is better than that of mechanical mixing molecular sieve.
2014, 31(5).
Abstract:A series of catalysts made of tungsten oxide loaded on SiO2, γ-Al2O3, and SiO2-Al2O3 were tested for esterification of acetic acid with ethanol. The catalysts were studied by characterization of XRD, nitrogen adsorption measurement, Raman and NH3-TPD in detail. The results indicated that tungsten oxide supported on SiO2-Al2O3 lead to the stronger and more acid sites, which appeared to be more effective for esterification of acetic acid with ethanol. Among these catalysts, SiO2-Al2O3 supported 8.0 wt% tungsten catalyst gave the highest activity for esterification of acetic acid with ethanol reaction with the conversion of acetic acid up to 69.7 %. Bulky crystalline WO3 loaded on SiO2-Al2O3 was disadvantage for improving activity of esterification.
ZHANG Xiao-juan , XIONG Shuang-li
2014, 31(5).
Abstract:In order to optimize the extraction process of heparin sodium and analysis the structure. This article used central composite design and response surface to optimize the extraction process of heparin sodium’s enzymatic method. The heparin sodium with high purity was obtained after the resinous adsorption, precipitator for deproteinization, alcohol precipitation and column chromatography for further isolation and purification. Agarose gel electrophoresis, infrared spectroscopy (IR), ultra violet (UV) spectrum and nuclear magnetic resonance (NMR) used to identify the structure of heparin sodium elementarily. The optimum extraction conditions are extraction temperature 53 ℃, extraction time 4h and pH 8.5. The crude and purified product extraction yield are 0.81 % and 0.05 %, the rough and depurated goods potency are 6.5 U/mg and 108.3 U/mg by the method of ovine plasma, respectively. An IR spectrum shows the characteristic absorption peaks are 890 cm-1 and 940 cm-1, UV spectrum displays the maximum absorption wavelength is 205 nm. Combined with agarose gel electrophoresis and NMR, the rarefied product is identified as heparin sodium.
SUN Shou-fei , DING Yun , YANG Huan , ZOU Chang-chang , QU Xiu-hong , REN Xiao-qian , WU Wen-liang
2014, 31(5).
Abstract:A series of phosphotungstic acid pillared Zn-Ti hydrotalcites(LDHs) were prepared by using the ion-exchange method. The structures of samples were characterized by XRD、FT-IR、SEM. The results showed that no significant structural change of LDH was observed after intercalation. The epoxidation of fatty acid methyl ester reactions were carried out over the catalyst samples. It was found that, 90.6% conversion of fatty acid methyl ester and 86.0% selectivity to epoxidation product could be obtained at the reaction temperature 70 ℃, reaction time 7 h, n(H2O2):n(double bond)=1.5:1, and catalyst dosage 7.0% (based on the weight of fatty acid methyl ester). The catalytic performance of phosphotungstic acid pillared Zn-Ti hydrotalcites was better than that of Zn-Ti LDH respectively. The novel phosphotungstic acid pillared Zn-Ti hydrotalcites catalysts revealed good catalytic performances to epoxidation of fatty acid methyl ester reactions. Furthermore, the pillared hydrotalcites showed a good repeatability after 5 times reuse.
2014, 31(5).
Abstract:6-Hydroxy-3,4-dihydro-2(1H)-quinolinone was synthesized by one-pot reaction of 4-methoxyaniline and acryloyl chloride using [bmim]Cl-AlCl3 ionic liquid as catalyst, and its structure was characterized and confirmed by IR, elemental analysis and 1H NMR spectra. Firstly, N-(4-Methoxyphenyl)acrylamide was obtained by acylation of 4-methoxyaniline using acryloyl chloride in [bmim]Cl-AlCl3. Secondly, with the cooperate catalysts of [bmim]Cl-AlCl3 and HCl produced by acylation, 6-hydroxy-3,4-dihydro-2(1H)-quinolinone was produced with a yield of 89.6% through intramolecular Friedel-Crafts alkylation and demethylation of N-(4-methoxyphenyl)acrylamide. As a task-specific ionic liquid, [bmim]Cl-AlCl3 plays the role as catalyst as well as solvent. And it can be recycled and utilized for five more times without significant decrease in the yield of the target compound.
zhangjing , maoguijie , WANG Ming-qi
2014, 31(5).
Abstract:Using substituted phenol as starting compound, through nucleophilic replace prepared substituted phenoxyacetate, then with silicone load stannic chloride, dimethylbenzene, 2-(Diethylamino)ethanol, six new (diethylamino)ethyl phenoxyacetate derivaties were synthesized. The title compounds were fully characterized by means of IR,1H NMR,13C NMR and MS. The preliminary results indicate that all these compounds can improve the nitrate reductase activity of the corn seedlings, under the concentration of 20 mg/L of the nitrate reductase activity of 2-bro-(diethylamino)ethyl phenoxyacetate was the highest.
2014, 31(5).
Abstract:Alkali isomerization of methyl linoleate by sodium hydroxide in ethylene glycol to prepare conjugated linoleic acid was explored. A conversion of methyl linoleate of 92.4 % and a yield of conjugated linoleic acid of 89.3 % were obtained under the optimum reaction conditions of m(sodium hydroxide): m(methyl linoleate): V(ethylene glycol) = 1: 5: 7.5 at 170 oC for 4 h. The advantages for the new alkali isomerization of methyl linoleate instead of linoleic acid are the low-cost for commonly used potassium hydroxide being replaced by sodium hydroxide, the low consumption of alkali as methyl linoleate instead of the facilely saponified linoleic acid, and the diminished consumption of ethylene glycol since the mass transfer is easy for less saponification initially occurred.
YAO Xiao-lei , XIONG Shuang-li
2014, 31(5).
Abstract:The porcine red blood corpuscle were hydrolzed by alcalase, the protein hydrolysate was prepared. The functional properties including protein solubility,emulsifying activity index(EAI)and emulsion stability index (ESI),foaming capacity and foam stability of protein hydrolysate were analyzed .Its antioxidant activity was also studied. The result showed that the protein hydrolysate had high water solubility,water adsorption,water retention ,medium foam formation, low stability for emusifying property and foam keeping. The molecular weight of it was distributed mainly over 2000~3000 . The studies on its antioxidant showed that protein hydrolysate had eliminating capability on •OH radical ,DPPH•radical ,lipid peroxidation, and also had significant total antioxidant capacity and chelating ability on ferrous ions.
2014, 31(5).
Abstract:With eight four methyl siloxane (D4), 1,3 -bis(3 -aminopropyl )-1,1,3,3 -tetramethyl disiloxane by bulk polymerization, the preparation of ammonia propyl sealing side polysiloxane (ASO - 2), then its and isophorone isocyanate (IPDI) and polyethylene glycol 1000 (PEG - 1000) and triethanolamine (TEOA) preparation of polyurethane pre polymers (PU) reaction, was IPDI type cationic waterborne polyurethane modified amino silicone finishing agent (PUASO - 2). Using IR, FE - SEM, nanometer particle sizer PUASO - 2 and its emulsion were studied. Research shows that: the outer emulsion prepared PUASO - 2 emulsion (PUAS - 2) particle distribution, the average particle size of 38.64 nm.When the polyurethane PU content of 20%, for cotton twill and plain cotton processing, respectively, after finishing the bending rigidity of 954 mN,525 mN, crease recovery Angle is 178.86 °and 272.81 °; Compared with not finishing two kinds of cotton fabrics, the growth of 23%, 26% and 37%,35% respectively。With ASO - 2 compared to the two kinds of cotton fabrics after finishing,PUAS - 2 to sort out the white degree of two kinds of cotton fabrics after wb increased to 78.18 wb and 73.45 wb from 81.13 wb and 76.64 wb, fabric crease recovery Angle increased by 140.44 ° and 205.65 ° respectively to 174.71 ° and 269.02 °, and static water absorption time increased to 1.78 s to 2.68 s, softness were slightly down.
2014, 31(5).
Abstract:A new quaternary ammonium modified amino polysiloxane (QASO-121)was synthesized by the quaternized modification of N,N-two methyl-γ-aminopropyl-γ-aminopropyl poly two methyl siloxane (ASO-121) using ethyl chloroacetate.The chemical structure of QASO-121,its emulsion and membrane configuration on fibers surface were characterized by infrared spectroscopy (IR),nuclear magnetic resonance spectroscopy (1HNMR),scanning electron microscopy (SEM),nanoparticle size analyzer and other instruments.The effects of its ammonia value,viscosity,pH and silicone emulsion dosage on the performance of treatment of cotton fabric were also discussed.The results show that the average particle size of the QASO-121 emulsion was 75.3 nm,potential was 21.2mV, and it had a good film-forming ability on fabric surface.The softness and hydrophilicity of fabric increased,the whiteness of fabrics remained the same,when the ammonia value of QASO-121 was 0.6 mmol/g,the viscosity was 2.600 Pa?s, the amount of the emulsion was 4g/L.Comparing the application performance of QASO-121 and not the quaternization of ASO-121,it is find that they had a similar effect on the softness of finishing fabric,but the finishing fabric using QASO-121 was full of elasticity and possessed the improved hydrophilicity,its yellowing resistence was also improved.
CAI Hong-yan , WANG Qiang , WANG Hong-zhuang , ZHANG Qun
2014, 31(5).
Abstract:Erucyl amidopropyl carboxyl betaine EBC was prepared from erucic acid, N,N-dimethyl-1,3-propanediamine, and sodium chloroacetate. The structures of erucyl amide EA and betaine product EBC were analyzed by FTIR and MS. Surface/Interface activities, adsorption characteristic and viscosifying capability of this surfactant were evaluated. The CMC of betaine EBC was 1.02×10-5 mol/L, and corresponding γCMC was 29.60 mN/m. The minimum carbon number of this betaine was 16. At alkali-free condition, ultralow interfacial tensions in the 10-4~10-3 mN/m magnitude were reached for betaine EBC with crude oil of Daqing and Sudan oilfields. In content range of 0.001%-0.20%, interfacial tension between EBC/DABS(8:2,wt%/wt%) combined formulation and crude oil of Changqing oilfield reached ultralow magnitude, showing excellent interfacial activity and strong anti-dilution capability. The adsorption on natural core sand of EBC was in 0.07~0.51 mg/g sand range, less than 1.0 mg/g evaluation criteria. In addition, solutions of this betaine exhibited good viscosifying capability. Erucyl amidopropyl carboxyl betaine EBC can be used as a suitable oil-displacement surfactant in combined chemical flooding.
MA Xi-ping , DAI Lei-yang , MA Qi-rui , SHI Hai-tao
2014, 31(5).
Abstract:This paper introduced a new zwitter-ion terpolymer through aqueous solution polymerization, which can be used in the drilling fluids. The monomers are acrylamide(AM),diallyl dimethyl ammonium chloride(DMDAAC) and sodium p-styrenesulfonate (SSS). A series of experimental factors were also discussed and the optimum scheme of copolymerization was obtained,that is,monomer mass is 25% ,temperature of reaction is 60℃ ,dosage of initiator is 0.5% ,molar ratio of monomer n(AM)∶n(DMDAAC)∶ n(SSS) is 8∶1∶1,reaction temperature is 60℃.The results of infrared characterization have confirmed that the structure of the product in question is consistent with the original design. The results showed that the product could control the fluid loss well and API could reach 7mL, otherwise it had inhibitory effect, which were worth popularization.
WU Zhan-min , ZHANG Shao-fei , HE Yu-feng , ZHAI Wen-zhong , WANG Rong-min
2014, 31(5).
Abstract:Firstly, the prepolymer of polyurethane (PU-HEMA) was synthesized using poly(propylene oxide glycol) (PPG), isophorone diisocyanate (IPDI) and dimethylol propionic acid (DMPA) as main monomers, and using hydroxyethyl methacrylate (HEMA) as grafting reagents. Then, using miniemulsion polymerization technology, the waterborne polyurethane - polyacrylate composite emulsion (PU-PA) was successfully prepared with copolymerization of acrylic ester and PU-HEMA. The effects of monomers dosage, ratio of PA/PU on the properties of PU-PA emulsion were investigated. It was found that the optimal dosage of DMPA, HEMA was 3 % and 6% respectively. The PU-PA was characterized by FT-IR, TG and SEM. The PU-PA was also applied to prepare waterborne polyurethane-acrylate composite coating (PU-PA-C) with the addition of pigments and fillers, such as diatomite, bentonite, etc. PU-PA-C meets the standard for interior wall coatings and architectural coatings. Its water absorption rate get to 206 %, and wash resistance is more than 900 times. The coatings showed strong performance of water absorption / desorption, which could be used as the interior wall coating in the building.
SU Kui , LIU Wei-qu , YAN Zhen-long , WANG Hong-lei
2014, 31(5):0-0.
Abstract:The polysiloxane containing unsaturated double bond has been synthesized by using silane coupling agent (KH570) which was hydrolyzed under pH=4 and terminal-hydroxyl polydimethylsiloxane which was prepared by octamethylcyclotetrasiloxane. And then, polyacrylate emulsion that modified by long chain branched polysiloxane containing unsaturated double bond was composed between (Meth) Acrylate and unsaturated long chain branched polysiloxane by free radical polymerization reaction. By this way, the amount of silicone in the copolymer can be achieved by 80%. The obtained polysiloxane containing unsaturated double bond and modified copolymer were characterized by means of FTIR, 29SiNMR. And also the properties of the emulsion and emulsion film were tested. The results shows that KH570 was fully hydrolyzed and then dehydrated with terminal-hydroxyl polydimethylsiloxane, which eventually made unsaturated long chain branched polysiloxane. It also shows that when mass fraction of silicone was 80%, water absorption eventually was 5.3%, and surface free energy was 6.56 mN/m, and the temperature of maximum thermal weight loss rate was 577℃. Hydrophobic property and thermal stability was improved greatly. So, the unsaturated long chain branched polysiloxane modified copolymer emulsion could be used as high hydrophobic and high heat resistant functional polymeric material.
PANG Jian-jun , ZHANG Li-ran , WANG Hao , ZHANG shu-xiong , WANG Dong-min
2014, 31(5).
Abstract:Five kinds of acrylic acid-co-sodium methallyl sulfonate(PC-1~5) were synthesized by free radical polymerization, and these copolymers′ influences on building gypsum system were studied, and compared with comb-like polycarboxylate-type(PC) and FDN. The results indicated that when the dosage was 0.3%: PC-4(nacrylic acid:nsodium methallyl sulfonate = 6:1) was the best copolymer on water-reducing rate, achieved 22%, and the longest slump retain,reached 70 min, and the lowest water absorption rate at 2h, achieved 16%, 11.5% lower than the blank, and the bending and compressive strength enhanced 30%, 31% respectively, and the highest softening coefficient, achieved 0.36, 0.1 higher than the blank. It was found that building gypsum hydration crystal form from needle turned to flake when added PC-4. The major functional groups of PC-4 was determined by IR. This shows that the adaptability of linear copolymer PC-4 on building gypsum system was fine.
2014, 31(5).
Abstract:Various acid/base compounds were used as catalysts for the synthesis of N-methyl methyl carbamate (MMC) from dimethyl urea (DMU) and dimethyl carbonate (DMC) in a batch reactor. The results showed that dibutyloxotin (DBTO) presented the best catalytic performance among the catalysts. The MMC structure was then confirmed by FTIR, 1HNMR and 13CNMR. Furthermore, effects of reaction conditions for the MMC synthesis over DBTO catalysts have been investigated. The optimal reaction conditions were as follows: DBTO 0.603 mmol,DMU 15.34 mmol, DMC 169.2 mmol, reaction temperature 423 K, reaction time 4 h, yielding MMC high to 99.96%.
2014, 31(5).
Abstract:Carfentrazone-ethyl was synthesized by one-pot reaction with 1-(5-amino-4-chloro-2- fluorophenyl)-4-(difluoromethyl)-3-methyl-1H-1,2,4-triazol-5(4H)-one(TZLO-A) as raw materials, copper(Ⅰ) chloride(CuCl) as catalyst and t-butyl nitrite(t-BuONO) as diazotized reagent through diazotization and Meerwin arylation reaction in acetonitrile or butanone. The structure of the product was characterized by 1HNMR、13CNMR and MS spectrum. The optimum reaction conditions of synthesis were obtained as follows: the molar ratio of TZLO-A, copper(Ⅰ) chloride, ethyl acrylate, to t-butyl nitrite was 1:(0.6-0.7):13.7:1.5, the adding time of hydrochloric acid and t-butyl nitrite was 20 min and 150 min respectively. Under these conditions, the target product was obtained with a yield of 92.9% and with a purity of 92%.
2014, 31(5).
Abstract:The iridium catalytic system composed of the [ IrHCl2( COD )]2 and the chiral diaminodiphosphine ligand was applied in the asymmetric transfer hydrogenation of 1,1-diphenylacetone in the synthesis of (S)-(-)-1,1- diphenyl -2-propanol. The influence of temperature, substrate/catalyst molar ratio, metal complex/chiral ligand molar ratio and lye concentration on the reaction was tested. The results show that 97.85% of yield and 99.35% ee were achieved when 1,1-dphenylacetone was reduced for 2 h in this catalytic system.
SUN Cai-ying , CHEN Peipei , WU Qiang , LI Qianwen
2014, 31(5).
Abstract:SPDPC was synthesized in Ion Liquid as solvent and catalyst. Pentaerythritol reacted with phosphorus oxychloride in 1:2.2 molar ratio under 40℃ for 7h,the yield is 66%. The structure of SPDPC was characterized by MP, IR and 1HNMR. The catalytic mechanism of Ion Liquid was speculated. The new way was compared with the traditional ones. It is found that Ion Liquid as solvent and catalyst not only shortened the time of reaction and reduced the reactive temperature, but avoided volatilizing, more collectable, economical and environmental friendly as a suitable solvent and catalyst for SPDPC synthesis.
2014, 31(5):0-0.
Abstract:As an important organic chemical material and monomer for producing epoxy resin, epichlorohydrin is industrially derived from the saponification cyclization of dichloropropanol in a tower reacting system. In order to separate product away speedy and effectively to depress energy consumption and wastewater discharge amount, tubular reactor coupling with thin film evaporation was designed as a new process for producing epichlorohydrin. The influence of different technical factors of the coupling process including reactants’ molar ratio, NaOH solution concentration, reaction temperature, tubular residence time, thin film evaporation temperature and thin film evaporation pressure on yield were investigated. It turned out that at conditions when n(NaOH): n(DCP) = 1.05:1, NaOH solution concentration at 20%(wt.), reaction temperature at 50℃, tubular residence time at 15s, thin film evaporation temperature at 50℃, thin film evaporation pressure at 100mbar, the yield of epichlorohydyin reached 97.3%. The coupling process of tubular reaction and thin film evaporation was improved in its lower material consumption, shorter reacting time and higher product yield. Comparing with tubular reactor - rectification coupling process, this process was superior for its better operation flexibility, higher product yield, lower energy consumption and lesser wastewater discharge.