2013, 30(2).
Abstract:A kind of high performance two-package automotive refinish was obtained with polyester resin modified acrylic-polyurethanes. The effect of acrylic resins, polyester resins and its amount, curing agent,the ratio of –NCO/-OH, leveling agents, anti-settling agent on film properties was studied. The results showed that the film had the best performance when the mass ratio of acrylic and polyester resin modified by CARDURA E10 (versatate glycidyl) was 5:1 ~ 3:1, N3390 was used as curing agent and the molar ratio of NCO/-OH was 1.08 ~1.15, the ratio of acrylic leveling agent and silicone leveling agent was 10:3, the quality percentage of anti-settling agent was 0.54%.
2013, 30(2).
Abstract:A novel proton-conducting monomer 4-[(3-(trimethoxysilyl)propoxy)methyl]-1H- 1,2,3-triazole(Ⅲ) was synthesized using chloromethyl pivalate as main materials by azide substitution, cycloaddition and Williamsen synthesis. The effects o f reaction temperature, reaction time, molar ratio of raw materials and ammount of catalysts on the yield were investigated by othorganol test and single factor experiments. The optimum reaction conditions for preparing azidomethyl pivalate(Ⅰ) were as follows: n(sodium azide ) :n( chloromethyl pivalate) =1.5:1, reaction time 20 h ,reaction temperature 78 ℃ and for preparing 2,2-dimethyl propionic acid-(4-hydroxymethyl-1,2,3 triazol-1-yl)methyl ester(Ⅱ) were: n(propargyl alcohol): n(Ⅰ)=1.3:1, reaction temperature 50 ℃, reaction time 24 h and n(CuSO4•5H2O):n(ascorbic acid):n (Ⅰ)=0.02:0.1:1. The yield of the product(Ⅲ) was 63.9%.The structures of the compounds synthesized were characterized by the methods of FTIR, 1H NMR and 13C NMR .
2013, 30(2).
Abstract:In this paper, the surfactivities of the water extraction of the Sapindus saponin from the pericarp of Sapindus mukorossi, its fermentation product, and the mixture of the fermentation product and other four surfactants were studied. Our results showed that, compared with the water extract, the stability at high temperature, lower critical micelle concentration(cmc) and surface tension(γcmc), foaming and emulsifying capability of the fermentation product were impoved in some degree. Based on Rosen theory, the binary mixture systems contained the fermentation product of Sapindus saponin and one of the follwing surfactants, Sodium alcohol ether sulphate(AES), Octadearyl dimethyl ammonium chloride(1831), Alkyl polyglycoside(APG), or Pepega, were constructured, and then their surfactivities were determined. According to the cmc, γcmc and foaming ability tests, they showed synergistic effects in different degree.In emulsifying ability test, a remarkable synergistic effect exsited in the mixture of the fermentation product/APG both on palm oil and liquid paraffin, while there were synergistic effects only on palm oil in the other three mixtures, not on liquid paraffin.
2013, 30(2).
Abstract:1,3-dihydroxyacetone was synthesized from paraformalclehyde by the catalysis of 3-ethylbenzothiazolium bromide under the protection of nitrogen with butyl alcohol as the dissovant and triethylamine as the cocatalyst. The effects of react temperature, react time and the amount of triethylamine on the yield of 1,3-dihydroxyacetone were investigated. The preferred synthesis parameters are as follows: the consumption of paraformalclehyde and catalyst is 60mmol and 3mmol respectively, the amount of triethylamine and butyl alcohol is 25mL and 10mL respectively, the react temperature is 130℃,the react time is 40min.The yield of DHA is 37%,the react selectivity is in the 95%-98% range.The purity of the product was increased from 90% to 99.8% after the purification processes of the successive esterification and hydrolysis separation,the total yield of DHA was 72% in the purification.The melting point of the product is 73℃.Its structure was confirmed via analysis of IR、1HNMR and ultraviolet visible spectrum.
GENG Long , LI Zhong-hui , GAO Wei , WU Qiu-fang , MA Xin-sheng
2013, 30(2).
Abstract:In this paper, 4, 4′-biphenol (BP) was prepared from waste LCP(PHBA- BP- PTA terpolymer)by hydrolysis process under atmospheric pressure using NaOH as catalyst, 1,4-dioxane and water as solvent.The effects of catalyst and solvent on hydrolysis reaction were studied. Under the optimum condition of reaction temperature 100˚C, reaction time 8 h and ratio of reaction mixture: m (LCP): m (solvent): m (H2O): m (NaOH) =1:4:1.5:0.6, the hydrolysis efficiency of the LCP is over 97%. With addition of HCl in the hydrolysate until pH=8.5, BP precipitation was formed. After BP was washed with water, dried and recrystallized in methanol, its purity could reach 99.9%. The yield of BP from the LCP is 70%.
2013, 30(2).
Abstract:Amplification experiments of preparing dodecyl glycoside in the 30ml reactor were founded in the lab. Effects of technological parameters on preparing stability were investigated. The acceptable product could not be gained according to the experimental conditions of small scale plant. Water content in the glucose, raw material ratio, dispersity in the raw material, and the stability of the technological parameters were all the main influence factors of amplification experiments. Experiments indicated that the best technological parameters were as follows. Glucose with no water must be sieved, premixed and batch fed. Raw material ratio was equal to 6:1. Temperature, pressure and so on, were automatically controlled by computer. Condenser and knockout drum were added to the vacuum plant. The accuracy and reliability of the method have been verified.
CHEN Haitao , ZHANG Ning , LIU Yang , CHENG Yue , SUN Bao-guo , ZHENG Fu-ping
2013, 30(2).
Abstract:Volatile flavor compounds from Jiayongxin preserved beef by accelerate solvent extraction-solvent assisted flavor evaporation(ASE-SAFE) and simultaneous distillation extraction(SDE), and identified by the gas chromatography-mass spectrometry.Results showed that a total of 84 compounds were identified and they were 6 hydrocarbons, 21 aldehydes, 10 alcohols, 11 ketones, 4 phenols, 16 acids, 3 ethers, 1 ester and 12 heterocyclic compounds, respectively. 16 compounds were all identified by the three solvents, involving hexanal,heptanal,benzaldehyde,nonanal,2-furanmethanol,linalol,α-terpineol, (-)-terpinen-4-ol, 1-hydroxy-2-propanone,acetoin,2,3-pentanedione, piperitone, eugenol, eucalyptol, anethole and dihydro-2-methyl-3(2H)-furanone, etc.
ZOU Xiao-yong , MU Zhao , ZHAO Ru-song
2013, 30(2).
Abstract:The stability of asphaltene model oil-in-water emulsion was studied using near infrared stability analyzer. The effect of two different surfactants(SDS and SDBS),the mass concentration of the asphaltene and the salt on the emulsion stability was investigated. The relationship between the interfacial tension and zeta potential and the emulsion stability was preliminarily studied. The results showed that the emulsion stabilized by SDBS was more stable than SDS, in the investigated range, the higher the mass concentration of the asphaltene was, the less stable the emulsion was, the salt can enhance the stability of the emulsion. The decrease of the interfacial tension is conductive to the stability of the O/W emulsion, while the zeta potential may not play an important role in keeping the stability of the emulsion.
2013, 30(2).
Abstract:By studying the volatile compounds of fermented soy sauces and acid-HVP under the optimized solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS) conditions, a novel method of identification of adulteration of soy sauces has been firstly proposed. The optimized SPME conditions were: adsorption time of 30 min, temperature of 50 ℃ and NaCl concentration of 100g/L. Totally, 11 and 15 characteristic compounds were screened in fermented soy sauce and acid-HVP, respectively. By excluding the possible interfering volatile compounds in caramel, 1-octene-3-ol was selected as the index of fermented soy sauces. 1-Phenyl-2-propanone was selected as the indexes of acid-HVP. The new judgment method was proposed and applied for the identification of commercial soy sauces.
2013, 30(2).
Abstract:The hyperbranched polyester with terminal hydroxyl groups was modified with maleic anhydride, and the hyperbranched maleate containing a great number of unsaturated double bonds in segmers was synthesized. The changes of viscosity, thermal stability and Tg on hyperbranched maleates with different modified degrees were analyzed and characterized. The hyperbranched maleates were used as prepolymer in UV-curable coating, and the effects of modified degrees on the adhesive strength, impact strength, flexibility, hardness and the solvent resistances of UV-curable coating were studied. The experiments indicated that the hyperbranched maleate was a kind of macromolecular material with low viscosity, good thermal stability and easy adjustable Tg. When the modified degree was 80%,the performances of the UV-curable coating were best, which the UV-curable time could reached 3s,the adhesive strength of coating was grade 1, impact strength was 48kgf.cm, the flexibility was above 7cm, the hardness reached 5H and it had the good solvent resistances.
2013, 30(2).
Abstract:The nanocapsule osmanthus/tuberose perfume condensed by ultrafiltration technology whose wall material is chitosan-sodium tripolyphosphate is investigated. A series of single factors were evaluated for analyzing the influence on time of concentration, diameter of particles, solid content and zeta potential for the best preparation conditions. The flavor-loaded nanocapsules were characterized by dynamic light scattering (DLS). Results showed the best preparation conditions are 150kD chitosan, 0.3MPa (pressure), 0.5% (content of perfume) for osmanthus nanocapsule; 150kD chitosan, 0.3MPa (pressure), 0.244% (content of perfume) for tuberose nanocapsule
2013, 30(2).
Abstract:Abstract:More than 99% purity of liquid crystal intermediate of 4-ethoxy-2,3-difluoroacetophenone was synthesized via Friedel-Crafts reaction with 2,3-difluoroethoxybenzene and acetyl chloride as starting materials. The target compound was characterized by 1HNMR、IR and GC-MS. The results of condition experiments showed the reaction effect was best with aluminium chloride as catalyst, dichloromethane as reaction solvent, when 2,3-difluoroethoxybenzene /aluminium chloride/acetyl chloride was 1/1.14/3,the reaction temperature was -10~-5 ℃ and the reaction time was 1 h. And the mechanism of Friedel-Crafts reaction and the generation cause of the by-products was speculated.
2013, 30(2).
Abstract:PVDF and PES-C blend membranes are prepared via TIPS method by using DBP and DMAc as mixed diluent. Membrane structure is observed and pure water flux is tested. Waste water treatment property is also checked in MBR. Compared with PVDF membrane, the blend membrane has a thinner skin layer and a porous support layer. Pure water flux of blend membrane is twice as much as that of PVDF membrane, at the same time, the blend membrane has higher sewage flux and higher remove ratio of COD and NH4+-N. The smaller flux attenuation coefficient of blend membrane represents a better antifouling property of it.
GAO Ji , LIU Jun-zhong , LI Hui , LIU Qian , JIAO Qing-cai
2013, 30(2).
Abstract:The serine deaminase from Escherichia coli K-12 MG1655 was recombinant expressed in Escherichia coli BL21 (DE3) using plasmid pET28a as vector. The enzymatic properties of recombinant serine deaminase were studied, and several influence factors of enzyme reaction such as temperature, initial pH, concentration of L-serine were investigated. Then DL-serine was resoluted with recombinant serine deaminase. The results indicated that the recombinant serine deaminase was successfully expressed, and the optimal conditions for enzymatic conversion of L-serine were 37oC, initial pH=9.0 and ? (L-serine) =4%. 0.3 g serine deaminase cell enzymatic conversion 100 ml ? (DL-serine) =8% needs 8 h, and the mole conversion rate of L-serine is up to 98%.
2013, 30(2).
Abstract:By the chemical reduction method, a series of NiWB catalysts were prepared and used for the transformation of microcrystalline cellulose by changing the concentration of the ammonium metatungsten(AMT). The influence of different ratio of Ni and W in the catalyst, the temperature, the pressure of H2, the reaction time and the catalyst dosage on the cellulose catalytic conversion was discussed. The results show that the appropriate conditions: the conversion of microcrystalline cellulose was up to 100% , the yield of ethylene glycol was 43% and the yield of hexitols was about 5% at 245℃, H2 pressure 6 MPa for 2h.
LIU Xiu-ying , pfcheng@.com , XU Wei-lin
2013, 30(2).
Abstract:Allyl methacrylate was synthesized from 3-chloropropene and sodium methacrylate with cetyltrimethylammonium bromide as the phase transfer catalyst. The products were characterized by IR, 1H NMR and the mass spectrometry. The effects of the reaction conditions on yields were investigated. The molar yield could reached 85% when the reaction conditions were as followings: the molar ratio of sodium methacrylate to 3-chloropropene was 1:2.5; the amount of catalyst and the polymerization inhibitor, p-benzoquinone, was 3 wt% and 0.5wt% of the sodium methacrylate, respectively; dimethyl sulfoxide was used as solvent and its volume was 2.25 times of that of 3-chloropropene; and the reaction was stirred at 50℃ for 3 hours.
GAO Kun , WANG Zhao-hui , WANG Xiao-zu
2013, 30(2).
Abstract:Zn-Mg-Al hydrotalcite nanoflake and Zn-Mg-Al hydrotalcite microstructure constructed by nanoflake had been synthesized via a hydrothermal condition at 120℃ for 10h with Zn(NO3)2、Al(NO3)3 and Mg(NO3)2 as reactants, using CO(NH2)2 as precipitation agent. The size, structure and morphology of as-prepared products were characterized by the XRD, FT-IR,TG-DTA,ICP and SEM, demonstrating that the as-prepared hydrotalcite has morphology of a homogeneous and regular flower-like structures with diameter of about 8μm and the measured thickness of the nanoflake is about 100nm and displayed excellent memory function. A possible formation mechanism of flower-like hydrotalcite was also discussed.
YAN Hui-qiong , LIN Qiang , LI Jia-cheng , FENG Yu-hong , HU Wen-tao , NIU Di
2013, 30(2).
Abstract:To obtain an acetamiprid pesticide carrier with high loading rate and good subtained-release properties,the acetamiprid hydrogel beads, which used bentonite as an adsorbent and film-forming properties of chitosan, were prepared by the extrusion-exogenous gelation method. And their structure, morphology and performance were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron micrograph (SEM), thermogravimetry (TG), water-up tests and release studies. Experimental results showed that the obtained hydrogel beads were 1.42~1.71mm in diameters. Bentonite could improve the hydrogel beads’ size and sphericity and make the drug loading rate and encapsulation efficiency of acetamiprid upgrade from 4.16% and 36.36% to 4.91% and 63.01%, respectively. Chitosan and sodium alginate had formed the polyelectrolyte complexes by electrostatic interactions assisting in crosslinking by calcium ion and made the drug loading rate and encapsulation efficiency of acetamiprid upgrade from 4.16% and 36.36% to 5.23% and 54.29%, respectively. Bentonite contains a lot of hydroxyl groups on the surface that could form the hydrogen bonds with the sodium alginate and chitosan, which could effectively inhibit calcium alginate large swelling to improve the performance of their release.
2013, 30(2).
Abstract:In this article, the 3-(diethoxymethylsilyl)propyl methacrylate (MPTS) were used as modified functional monomer, acrylic ester and acrylic acid as main monomers, ionic emulsifiers and nonionic emulsifiers as the composite emulsifier, persulfate(KPS) as initiator, and the slicone modified acrylate copolymer emulsion (SAE) was successfully prepared. The relationship between stability of SAE emulsion and contents of MPTS, ?-hydroxypropyl methaerylate (HPMA), initiator and copolymerization temperature were investigated. IR and TG was used to characterize SAE. The SAE copolymer emulsion was applied to prepare the silicones-acrylate copolymer humidity coating (SAE-C) with adding pigments and fillers, such as diatomite, bentonite, etc. Based on measuring the basic performance of copolymer emulsion film and SAE-C coatings, the humidifying function of SAE-C coating was investigated. In conclusion, MPTS could improve the adhesion of SAE film and water resistance of the coating. The results showed that the basic properties of SAE and the SAE-C match the standard for interior wall coatings. The obtained coatings had good humidity-sensitivity and humidity retention, which could be used as the interior walls coating in the building.
WANG Fang-ping , MU Hu-po , ZHANG Jun-ying , LI Wan-xia , WANG Qi-zhao , DU Xin-zhen
2013, 30(2).
Abstract:A pH-sensitive PAA-co-octylphenyl polyoxyethylene methacrylate hydrogel[P(AA-co-C8PhEO10Mac)] was synthesized by free radical crosslinking polymerization, Swelling property, swelling and deswelling kinetics of the hydrogels in different pH media werestudied and hydrogel microstructures were investigated by means of scanning electron microscopy(SEM). L-ascorbic acid was chosen as a model drug and the controlled-release properties of hydrogels were pilot studied. The results showed that the P(AA-co-C8PhEO10Mac) hydrogel has a porous structure, both the rapid swelling and deswelling rate, good pH sensitivity characteristics; The swelling ratios of the gels in stimulated intestinal ?uids (SIF, pH=7.4) were higher than those in stimulated gastric ?uids (SGF, pH=1.4).With an increase of the content of acrylic acid, the swelling ratios of gels increased first and then decreased.The inhibitory effects of C8PhEO10Mac on escherichia coli and saccharomyces cerevisiae were sthdied, the results indicate that C8PhEO10Mac has no effect on them in the 10~50mmol/L test level.
HE Zhi-qiang , ZHU Zong-li , FANG Yun , Sun Suoshuang
2013, 30(2).
Abstract:Methylene bisalkylphenols were synthesized by condensation reaction from alkylphenol and formaldehyde in an oxalic acid-catalyzed autoclave process, and the target products were identified by IR, ESI-MS and 1H-NMR. The experimental results showed that compared with normal pressure process autoclave process made the conversion of nonylphenol increased about 20 % and the selectivity of methylene bisnonylphenol elevated approximately 10 %. The effect of catalyst dosage, reaction time, temperature and substrate molar ratio on the condensation reaction were investigated one by one, and thus the conversion of nonylphenol was further improved and the selectivity of methylene bisnonylphenol was as high as 92.1 %. The condensation conditions for preparing methylene bisdodeylphenol in an autoclave process also were optimized by an orthogonal experiment. The experimental results showed that the autoclave process is a facile, low-cost and efficient technology to synthesize methylene bisalkylphenols, the precursor hydrophobic skeletons of Gemini surfactants.
2013, 30(2).
Abstract:2-(4-hydroxy-phenyl)-1,1,1,3,3,3-hexafluoro-propan-2-ol (1) was obtained from 2-(4-amino-phenyl)-1,1,1,3,3,3-hexafluoro-propan-2-ol (2) via diazotization and hydrolysis; The influence factors of diazotization and hydrolysis were investigated. The product was identified by EA, 1H NMR, IR and MS spectra. The results showed the optimum reaction conditions were as follows: during diazotization, w(H2SO4)=w(NaNO2)=30%, n(H2SO4) : n (NaNO2) : n (1) = 4.0 : 1.1 : 1.0, reaction temperature -2~2 ℃; during hydrolysis, w(H2SO4)=50%, n (H2SO4): n (1) = 11: 1.0, reaction temperature 108~112 ℃ and reaction time 2 h. Under these conditions, 91% 2-(4-hydroxy-phenyl)-1,1,1,3,3,3-hexafluoro-propan-2-ol was obtained.
2013, 30(2).
Abstract:The aim of this paper was to obtain pure mono-hydroperoxide of trilinolein, which was a substance we required for the investigation of the mechanism of meat flavor formation via the technology of controlled fat oxidation combined with the thermal reaction. The material containing mono-hydroperoxide of trilinolein was prepared by oxidization of sunflower oil at 70 oC for 70 h with air ventilated at 0.72m3/kg?h, whereby the percentage of mono-hydroperoxide of trilinolein in the resulting oxidized sunflower oil was 1.95% identified by HPLC-MS and quantified by HPLC-ELSD. High-speed counter-current chromatography (HSCCC) was utilized for separation and isolation of mono-hydroperoxide of trilinolein from the oxidized sunflower oil. The optimum two-phase solvent system selected was n-hexane-dichloromethane-acetonitrile (4:1:3, V/V/V). With the upper phase of the two-phase solvent system as the stationary phase, and the lower phase as the mobile phase, the mobile phase was eluted in the normal direction at a flow rate of 1.5 mL/min while the revolution speed was set at 850 rpm/min. By the above conditions, 53 mg of mono-hydroperoxide of trilinolein was obtained in 195 min in one run from 5 g of the oxidized sunflower oil in a purity of 96.3% analyzed by HPLC-ELSD, and the recovery was 52.3%.
2013, 30(2).
Abstract:2-(1,1,2,3,3-Pentamethylindan-5yl)propanol (commonly known as indanol) was synthesized by the reaction of 1,1,2,3,3-pentamethylindane with propylene oxide, catalyzed by anhydrous AlCl3 using dichloromethane as solvent. The product was purified through ultrasonic assisted dissolution-crystallization process. Effects of mole ratio of 1,1,2,3,3-pentamethylindane to propylene oxide, amount of anhydrous AlCl3 and reaction temperature were investigated. The selectivity of indanol was 99% under the following reaction conditions: reaction temperature was -10℃~-15℃, n (pentamethylindane):n (propylene oxide):n (anhydrous AlCl3) was 1:1.2:1.2, and the reaction time was 2 h. The conversion of 1,1,2,3,3-pentamethylindane was 55.8%.The purity of indanol was 99%. The peculiar burnt smell originated from the distillation process was avoided in this purification process. The structure of indanol was characterized by data of FTIR, GC-MS, HRESIMS, elementary analysis, 1H NMR and 13C NMR spectrum.
2013, 30(2):0-0.
Abstract:A series of para-substituted 1,3-diphenyl-1,3-propanedione compounds have been synthesized by the Claisen condensation reaction of different substituted aromatic ketone and ester. Experiment based upon orthogonal design with four factors and three levels was carried out for optimization of conditions for 1,3-bis-(4-Methoxy-phenyl)-1,3-propanedione. Experimental results showed the suitable conditions as follows:using toluene as solvent and sodium amide as catalyst, n(p-methoxy acetophenone):n (methyl-p-methoxybenzoate):n (sodium amide ) = 1:4:5. microwave irradiation power was 320W and reaction time 45min. The yield can achieve 72.1%.The structures of synthetic products were characterized by IR and 1HNMR .HPLC was selected to determine the concentration of products. The products are good UV ultraviolet absorbents and exhibit significant antioxidation activity on lard..
CHEN De-li , SUN Yu-wan , LIU Ping-huai
2013, 30(2):0-0.
Abstract:Identified liposoluble extractⅠand Ⅱfrom Drypetes hainanensis fruit by GC-MS, which were isolated by solvent extraction method and silica column chromatography. The results showed that the main constituents of the extractⅠconsisted of bis(2-ethylhexyl) phthalate (64.2%) and alkanes (23.7%) etc. 19 compounds were found in the extractⅡ, mainly comprised olefin (1.4%), alkanes (22.9%), esters (67.9%) and phytol (2.8%) etc. The esters mainly concluded saturated fatty acid ester (35.7%), which was composed of hexadecanoic acid, methyl ester (29.0%) and octadecanoic acid methyl ester (6.8%), unsaturated fatty acid ester (18.6%), which was constituted by methyl 11,14-octadecadienoate (10.1%) and 6,11-eicosadienoic acid, methyl ester (8.5%), additionally contained bis(2-ethylhexyl) phthalate (13.6%).