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2008 Vol.25 Issue.4,
Published 2008-07-15
Article
Article
283
Quantitative Analysis and Observation of the Convection near Gas-Liquid Interface
LIU Chang-xu,ZENG Ai-wu,YU Guo-cong
By utilizing the method of Schlieren system,interfacial turbulence of convective structure in desorption of ethanol from water was observed and quantitatively analyzed.Horizontal unstable gas-liquid mass transfer experimental equipment was set up.The Marangoni interfacial convective structures caused by gas-liquid mass transfer in the interface during the desorption process of ethanol aqueous solution were observed.By employing the improved Schlieren,the concentration gradient of vicinity interface during gas-liquid mass transfer process was obtained. The quantitatively experimental result showed that the reason that induces the Marangoni convection is the local large surface tension gradient along the interface of the gas and liquid.This successfully explains the chaotic flow patterns obtained in gas-liquid mass transfer process accompanied by Marangoni effect and is helpful for the further study on the interfacial turbulence phenomena.
2008 Vol. 25 (4): 283-288 [
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1831
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Synthesis and Characterization of β-cyclodextrin Supramolecular Complexes
JIANG Hui-ming~
Supramolecular complexes between β-cyclodextrin and anthrone,butyl acrylate,triethylamine were synthesized and characterized by means of(()~1H-NMR) technique.Via molecular calculations,the possibilities of forming sumpramolecular complexes were verified.The possible conformations of the guest molecules inside the cavity of β-cyclodextrin were depicted through NMR analysis.
2008 Vol. 25 (4): 289-293 [
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2100
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294
Mechanism for Impurities Forming During the Synthesis of DNS and Optimization of DNS Preparation
CHANG Gui-xia~
The oxidation of p-nitrotoluene-2-sulfonic acid to prepare 4,4′-dinitrostilbene-2,2′-disulfonic acid(DNS) was monitored,and the mechanism for the formation of by-products 4-nitrobenzaldehyde-2-sulfonic acid (NBS) and 4-nitro-2-sulfobenzonic acid(NSB) was suggested.By investigating the influences of temperature,pH value,recrystallization times and solar light on the purity and recovery of DNS,optimized conditions for the recrystallization of DNS were obtained: about 85 ℃ and pH=9—10.Finally,4,4′-diaminostilbene-2,2′-disulfonic acid(DSD) with high quality was synthesized from DNS after purification.
2008 Vol. 25 (4): 294-297 [
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298
Reduction of DNS to DSD Acid by Hydrogenation
WANG Jue~1,QIN Zhi-zhong~2,ZHANG Guo-liang~1,ZHANG Feng-bao~1
4,4′-diaminostilbene-2,2′-disulfonic acid(DSD acid) was prepared via reduction of 4,4′-dinitrostilbene-2,2′-disulfonic acid(DNS) with liquid-phase catalytic hydrogenation method using Raney nickel as catalyst in water medium.The optimum technical conditions determined by a series of experiments were as follows:the concentration of DNS is 150—175 g/L,the amount of the catalyst used preferably 4% by weight based on DNS,temperature is 45—50 ℃,hydrogen pressure is 0.8 MPa.Under these optimum technical conditions,the purity of the product comes up to 98.4%.
2008 Vol. 25 (4): 298-301 [
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302
Synthesis of Organic Pre-sulfurizing Agent
WANG De-qiu~1,DONG Qun~1,ZOU Dan~2,JI Yong-gang~1
Polysulfides was synthesized using FCC gasoline and sulfur.Suitable catalyst was selected,the effect of catalyst mass,mole ratio of sulfur to FCC gasoline,reaction temperature and reaction time on the sulfur content of product were investigated.The optimum conditions were: mole ratio of sulfur to FCC gasoline is 2.0,reaction time,2.0 h,reaction temperature,170 ℃,mass ratio of catalyst to FCC gasolines is 0.05.The product obtained has high sulfur content,wide decomposation temperature and low viscosity.
2008 Vol. 25 (4): 302-305 [
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1960
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306
Synthesis of t-butyl-p-cresol with Supported HPWA/SBA-15 Catalyst
WU Bing~1,SHEN Jian~1,LI Hui-peng~1,FENG Jian~2
SBA-15 molecular sieve modified by HPWA were prepared and used to sythesize 2t-butyl-p-cresol by the alkylation of p-cresol with MTBE.The catalytic performances of the catalysts were studied in a micro-reactor.The influences of the content of hydrofluoric acid,reaction temperature,space velocity and mol ratio of MTBE to p-cresol on the conversion and the selectivity were analyzed.The results showed that the increasing conversion was attributed to the increase of acidity.The optimum conditions were:phosphotungstic acid is 40%,160 ℃ and the space velocity is 3.0 h~(-1), mol ratio of MTBE to p-cresol is 1.5.The conversion of p-cresol was 65.87%,and the selectivity of 2-t-butyl-p-cresol was 97.81%.
2008 Vol. 25 (4): 306-309 [
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310
Synthesis Technics of Thymosin α_1 by Solid Phase Convergent Peptide
WANG Wei,ZHANG Hong-peng,HUANG He
Based on solid-phase peptide synthesis,thymosin α_1(Tα_1) was synthesized by solid phase convergent synthesis.The effects of convergent protocol,coupling time,coupling solvents,coupling reagents and acetylation ways on the yield of Tα_1 were studied.The optimal protocol was obtained.Using the sequential condensation of three protected peptide segments(1—10,11—18,19—28),20.0 h as the coupling time,mixture of V(DMF)/V(DCM)=3.0 as the coupling solvent,HATU as the coupling reagent,the yield of crude thymosin α_1 was 64.3% with a purity of 61.1%.Compared with solid-phase peptide synthesis,the purity of thymosin α_1 synthesized by solid-phase convergent synthesis was increased by 29.9%.
2008 Vol. 25 (4): 310-313 [
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314
Pyrolysis of Polytetrafluoroethylene
LIANG Xuan-xuan,ZHANG Xiao-ping
The pyrolysis characteristics of polytetrafluoroethylene(PTFE) were studied in the atmosphere of nitrogen by thermogravimetric analysis.The results showed that the pyrolysis of samples has similar TG and DTG curves with the different heating rates.The pyrolysis of PTFE is an endothermic reaction.There is only one weight loss step including a weight loss peak in the entire process of the pyrolysis.The detection of gas products was performed by the coupled simultaneous Fourier transform infared spectroscopy.The experimental results showed that the principal product of the pyrolysis is tetrafluoroethylene.In addition,the element composition of the pyrolysis remnants was analyzed by electron probe.The analytical results indicated that the metal content of the remnants is close to that of ordinary stainless steel.
2008 Vol. 25 (4): 314-318 [
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319
Synthesis and Characterization of Bis(2,4-di-tert-butyl-phenyl) Pentaerythritol Diphosphite
PAN Zhao-qun,KANG Ying-zi
Bis(2,4-di-tert-butyl-phenyl) pentaerythritol diphosphite(antioxidant 626) was synthesized with pentaerythritol,di-tert-butylphenol and phosphorus trichloride.The effects of reaction temperature,reaction time,catalyst and the molar ratio of raw materials on the yield of the product were discussed by orthogonal experiment.From the experimental results,the optimized conditions were obtained.The first reaction was carried out at 55 ℃ for 3 h,while the second reaction at 125 ℃ for 2 h.The molar ratio of pentaerythritol,phosphorus trichloride and di-tert-butylphenol is 1∶2.05∶2.0,and the weight ratio of catalyst B to pentaerythritol is 0.022.The element analysis and IR spectrogram of the product agreed well with the target product.
2008 Vol. 25 (4): 319-323 [
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324
Synthesis and Thermal Decomposition Kinetics of Hydrargyrum 2-Mercaptopyridine
LU Lian-ying,WANG Dun-jia
2-mercaptopridine base derived Hg(Ⅱ) complex was synthesized.The complex was characterized by elemental analysis,titration analysis and IR.The thermal decomposition of hydrargyrum 2-mercaptopridine and its non-isothermal kinetics were studied by TG-DTG technique.The TG-DTG curves showed that its thermal decomposition was two-step process.The mechanism function and kinetic parameters of the thermal decomposition in the first step were obtained.Chemical reaction mechanism(F2) controlled the first thermal decomposition process.The kinetic equation may be expressed as: dα/dT=A/β·e~(-E/RT)(1-α)~2.The apparent activation energy and the pre-exponential factor were 189.67 kJ·mol~(-1) and 3.79×10~(18) s~(-1) respectively.
2008 Vol. 25 (4): 324-327 [
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2065
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328
Green Design Analysis of Amlodipine Maleate Refined Processes
CHEN Li-qun
Conceptual green design for the methanol solvent and the tail gas recovery in refined process in the production of Amlodipine Maleate were carried out.The advantage and disadvantage of several kinds of dryness,solvent recovery processes and equipment were compared.Through green design,products with good function,life cycle and good quality were obtained,and the influence of the process on the environment was reduced.
2008 Vol. 25 (4): 328-334 [
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335
Effect of K,Zr on the MoS_2/C Catalyst for the Synthesis of Ethyl Acetate from the Dehydrogenation of Ethanol
WANG Da-lin,YUAN Fa-lin,JIANG Hao-xi
The effect of K and Zr on the performance of MoS_2/C catalyst for the synthesis of ethyl acetate from the dehydrogenation of ethanol were study by XRD,XPS and catalyst activity measurement.The results show that the addition of K restrained the dehydration of ethanol to produce the ethylene and increased the united selectivity;Zr increased the conversion of ethanol;the simultaneous addition of K and Zr increased both of conversion of ethanol and united selectivity;the addition of Zr and K-Zr considerably influence the valence of Mo in the catalyst.
2008 Vol. 25 (4): 335-339 [
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340
Crystal Structure Prediction of 5′-GMP
LIU Mei,WEI Hong-yuan
The crystal structure prediction of 5′-GMP was performed using Polymorph in Cerius~2.A fast and reliable Monte Carlo simulated annealing process(MC-SA) was used to search for probable crystal packing alternatives on lattice energy hyper-surface;Optionally,these potential structures were clustered into unique groups based on packing similarity.The geometry of each unique structure was optimized with respect to all degrees of freedom or with rigid body constraints where the relative distance between a group of atoms are fixed;the optimized structures were clustered again to remove duplicates;the final structures were ranked according to lattice energy.Finally,the most likely stable space group of 5′-GMP was found to be P2_12_12_1.
2008 Vol. 25 (4): 340-343 [
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Review on the Synthesis of the New Antivirus Agent Valganciclovir
LIU Qiao-yun,ZHAO Hui-shuang,CHEN Wen-hua
Valganciclovir is a prodrug of Ganciclovir which has been newly developed for the treatment of cytomegalovirus(CMV) retinitis in patients with Aids.The bioavailability of oral Valganciclovir is higher than Ganciclovir while the toxicity is lower,so it has a wide market prospect.In this paper,synthetic methods of Valganciclovir were analyzed and compared with each other,and the merits and defects of each method were presented.
2008 Vol. 25 (4): 344-348 [
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349
Progress in Mesoporous Catalysts for Isomerization of High n-Alkanes
GUO Hai-feng,DONG Qun,HU Yun-feng
The catalysts for selective conversion of high n-alkanes into their branched isomers were introduced,particularly the mesoporous materials.With the development of mesoporous materials,many kinds of mesoporous materials with different components and structures were synthesized by different cooperative assembly pathway and at different synthesizing conditions. The ordered mesoporous catalysts were modified,and were testified with good activity and selectivity for selective conversion of high n-alkanes into their branched isomers.Some of the results have been applied in the oil refining and petrochemical industries.
2008 Vol. 25 (4): 349-352 [
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1911
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2759
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353
Development of the Nanocomposite Gel Polymer Electrolyte
WANG Shu-hui,YAN Hong-xia,MA Xiao-yan,HUANG Yun
The categories and properties of inorganic nanofillers,such as metal oxide,nonmetal oxide and clay,which are used to modify gel polymer electrolyte were reviewed.Based on these the influence of inorganic nanofillers on the properties of gel polymer electrolyte was analyzed.
2008 Vol. 25 (4): 353-358 [
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359
Application of Niobic Acid in Catalysis
LI Chun-jing,SHEN Jian
Niobic acid and compounds containing niobium are applied in a wide range of catalysis fields for their unique acidic property and thermal stability.Niobic acid as a solid catalyst can be directly applied in the hydrolysis,esterification,condensation and alkylation reaction etc.Compounds containing niobium,as a supporter loaded metal,can be used in Fischer-Tropsch synthesis,hydrogenation and oxidation reactions etc.As a supported catalyst,it can be loaded to different type of catalysts.Compounds containing niobium can also be widely used in a variety of chemical reactions as assistant or photocatalysts.The niobium catalysts had high catalytic activity,selectivity and long service life,so the development of new type of niobium catalysts has a good prospect.
2008 Vol. 25 (4): 359-364 [
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365
Independent Innovation Capacity and Policy Suggestions for Petrochemical Industry of China
CAO Yan,PANG Jing-an
According to China statistical yearbook on science and technology(2006)"Statistical Data on Independent Innovation of Chinese Big and Medium Sized Industrial Enterprises" promulgated by the Bureau of National Statistic,the R&D activities of petrochemical industry and their sub-industries under a set of appraisal index system,were evaluated and the independent innovation ability of these industries were analyzed based on real data.Furthermore,suggestion were provided to the relative administrative institutes in reinforcing the independent innovation ability in petrochemical industry.
2008 Vol. 25 (4): 365-369 [
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1798
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370
Vapor-Liquid Equilibria for Dimethyl Carbonate-Benzyl Alcohol System
GAO Jun,QU Peng-fei,WANG Zhong-wei,DAI Zhi-feng,JIA Mei-xin
Vapor-liquid equilibria(VLE) data of dimethyl carbonate(DMC)(1)-benzyl alcohol(2) system at 101.33 kPa were measured.The thermodynamic consistency of the VLE data was examined by Herrington method.In the meantime,the infinite dilution activity coefficient of dimethyl carbonate and benzyl alcohol and the parameters of activity coefficient of Wilson model were determined with the experimental data.The isothermal vapor-liquid equilibria data at 413.15 K were predicted.
2008 Vol. 25 (4): 370-372 [
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1974
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373
Purification of Tea Saponin from Methanol Phase Using Macro-Porous Resins
ZHU Bing~1,CHEN De-jun~1,QIAN Ren-yuan~2
Tea saponin was purified from methanol phase using macroporous resins in static state,different factors during the adsorption and desorption process were studied,such as pH,tea saponin concentrations,temperature,time.The optimal operation conditions were established.The resins adsorption capacity is 145.45 mg/g,the desorption rate is 90%.
2008 Vol. 25 (4): 373-376 [
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377
2008 Vol. 25 (4): 377-377 [
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