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2006 Vol.23 Issue.5,
Published 2006-09-15
Article
Article
377
Continuous Synthesis of Ethyl Butyrate by Reactive Distillation
WANG Hao-shui~1,XU Ding-wang~2,JIN Si-yi~2
Catalyzed by p-toluene sulphoric acid,continuous synthesis of ethyl butyrate by reactive distillation method was performed with experiment and computer simulation.Based on the results of the Aspen Plus simulation and experiment of the reactive distillation column,the process simulation and experiment were carried out and the feasible process scheme was proposed.By this technic,the theoretical content of the ethyl butyrate in the product could reach 99.5%.Also,the proposed technic has the advantages of more simple,less waste water letting off,and lower investment etc.
2006 Vol. 23 (5): 377-381 [
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1838
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382
Preparation of Nano-meter Photocatalytic Compound of TiO_2/SnO_2 and Its Degradability of the Pesticide Waste of Parathion
HUANG Li,ZHANG Hao,TAN Xin
Based on preparation of SnO_2 sol by sol-gel method,nano-meter photocatalytic compound of TiO_2/SnO_2 was prepared and the atom ratio of titanium to tin on the surface is 85∶15(by XPS analysis).The photocatalytic compound was used to degrade the pesticide waste of parathion and the experimental results indicated that the photocatalytic activity of photocatalytic compound is higher than that of TiO_2.Probably the reason is that the SnO_2 in TiO_2/SnO_2 photocatalytic compound formed the transferring place for electron,decreased the composition of electron-cavity,then enhanced the photocatalytic properties of the photocatalytic compound.
2006 Vol. 23 (5): 382-384 [
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2607
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385
Preparation of β-Bromoethyl Benzene by Anti-Markovnikov Addition of Hydrogen Bromide to Styrene
ZHANG Tian-yong,XU Dan,FU Qiang,ZHANG You-lan
β-bromoethyl benzene(β-BEB) was synthesized by anti-Markovnikov addition of hydrogen bromide to styrene.The reaction conditions such as the reaction time,the amounts of solvent and radical initiators,and the reaction temperature were studied.Finally,the product was analyzed by gas chromatographic analysis.Under the optimum reaction conditions that HBr was 1.2 mole of styrene,the volume of heptane was 5 times of styrene,the mass percentage of azobisisobutylnitrile(AIBN) was 0.5% of styrene,the reaction temperature was(80 ℃) and the reaction time was 60 min,the yield of β-BEB ≥92.0% and the purity ≥96.8%.
2006 Vol. 23 (5): 385-388 [
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3124
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6696
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389
Composition and Performance of Membrane Electrode Assembly in PEMFC
SHI Zhao-yuan~1,TIAN Jian-hua~1,SHI Jin-song~1,LIANG Bao-chen~2
The membrane electrode assembly(MEA) in proton exchange membrane fuel cell(PEMFC) was composed of the proton exchange membrane,catalyst layer,water management layer(WML) and diffusion layer.The influence of the thickness and polytetrafluoroethylene(PTFE) content of WML on the performance of MEAs was studied.Two kinds of new pore-forming agents,NH_4HCO_3 and(NH_4)_2SO_4,were used to optimize the pore structure of WML.The pore structure and surface appearance of WML were investigated by the environmental scanning electron microscopy(ESEM) method.I-V characteristic of the MEA was tested under conditions of the external humidification and self-humidification.The results showed that the MEA with WWL exhibited a better ability of water management and an improved I-V characteristic under conditions of self-humidification.
2006 Vol. 23 (5): 389-392 [
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1744
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3311
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393
Design of Control System in Enzymatic Membrane Reactor
WU Yu-feng,YANG Xue-you,HE Ming-xia,ZHANG Xu,SAN Hong-liang
A solution of continuous respond in the control of the enzymatic membrane reactor is proposed.The temperature,pH value and volume of liquid in the reactor are real-time measured by single chip computer and auto controlled to satisfy with continuous respond of the enzymatic membrane reactor.Experiments have shown that the conversion and yield of the product have been improved and this method can be generalized a lot.
2006 Vol. 23 (5): 393-395 [
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1669
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2640
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396
Synthesis of Chiral 4-Piperidones
SUN Ju-feng,CHEN Li-gong
Piperidones and its derivatives are a class of compounds with pharmaceutical and agricultural importance.Several new chiral compounds of N-substituted 4-piperidones were obtained from chiral reagent hydroxylamines and methyl acrylate.Their structures were proved by()~1H NMR and()~(13)C NMR.
2006 Vol. 23 (5): 396-399 [
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1678
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3116
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400
MoS_2/C Catalyst for One-Step Synthesis of Ethyl Acetate from Ethanol
CUI Neng-wei,LIU Cheng,JIANG Hao-xi,ZHANG Min-hua
A new MoS_2/C catalyst for one-step synthesis of ethyl acetate from ethanol was proposed.The effects of ATTM loading quantity on the performance of MoS_2/C catalyst were investigated and the results indicated that when the best loading quantity was 20%,the ethanol coversion was 88%,the acetate selectivity was 48%,the combined selectivity of ethyl acetate and aldehyde was 85%.The higher loading would decrease ethanol conversion and ethyl acetate selectivity.The preliminary mechanism was proposed based on the experiment,the proposed reaction mechanism was that ethyl acetate was produced via dehydrogenation of ethanol and acetaldehyde.
2006 Vol. 23 (5): 400-402 [
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1690
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3535
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403
Synthesis and Characterization of 2′,7′-Dichloride-5(6)-Fluorescein Isothiocyanate
PAN Hui-ying,GE Feng-yan,CHEN Li-gong
Fluorescein isothiocyanate(FITC) is an important fluorescence probe.In this paper 2′,7′-dichloride-5(6)-fluorescein isothiocyanate was obtained from 4-nitrophthalic acid,4-chloride-resoreinol and zinc chloride through condensation,reduction and isothiocyanatation in a total yield of 34.78%.The structure of the products were characterized by()~1H NMR,()~(13)C NMR,IR and MS,and the fluorescent properties of the products were determined.The results showed the fluorescent properties of the products were prior to that of FITC.
2006 Vol. 23 (5): 403-406 [
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1978
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1901
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407
New Process for Producing Thiourea from Urea
QI Xin,WANG Qian,LI Zhong-bo,LI Wen-feng
A new process,urea-calcium cyanamide method,for producing thiourea from urea and hydrogen sulfide is proposed.Calcium cyanate is prepared from urea and cium cyanamide and hydrogen sulfide.Thiourea is refined by freezing crystallite.The experimental results indicated that by this process,the production can reach the standard of country,and the yield is 5%—10% more than that of the old process.
2006 Vol. 23 (5): 407-410 [
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411
Gas-Agitated Liquid-Liquid Extraction of Hydrogen Peroxide
LIU Chuan-qiang~1,MA Zhong-long~2,JIANG Shao-kun~1,LIU Jian-guo~1
In a plate column with diameter of 50 mm,the process of gas-agitation extraction about anthraquinone working solution-H_2O_2-H_2O system has been studied.The system temperature maintained at 40 ℃.The air superfacial velocity was 0—3.22 mm/s and the disperse phase superficial velocity was 1.27—1.70 mm/s.The superficial flow ratio of dispersed phase to continuous phase was maintained at 50∶1.The experimental result showed that the overall plate extraction efficiency of gas-agitated plate column is obviously higher than that of conventional plate column,disperse phase hold-up increased and the content of hydrogen peroxide in residual extraction decreased.
2006 Vol. 23 (5): 411-414 [
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2191
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2158
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415
Correlation and Determination of Densities and Viscosities for Binary Mixture of the Cyclohexanone with Cyclohexane at Different Temperature
XIANG Zheng-le,MA Pei-sheng,FENG Li-mei,YANG Chang-sheng
Densities and viscosities of the binary mixtures of cyclohexanone with cyclohexane were determined between 293.15 and 343.15K under atmospheric pressure using a vibrating U-shaped sample tube densimeter and Ubbelohde suspended-level viscometer.Densities and viscosities of solutions were used to calculate excess molar volumes and excess viscosities respectively.The excess molar volumes are positive and the excess viscosities are negative.Excess volumes and excess viscosities were correlated by the Redlich-Kister equation respectively.The maximum standard deviations were lower than 3%.The results show this system can be regressed by using Redlich-Kister equation.Viscosities of cyclohexanone and cyclohexane mixtures were correlated with temperatures by the Andrade equation.The correlation coefficients approximate to 1.
2006 Vol. 23 (5): 415-419 [
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2382
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249KB] (
3586
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420
Measurement and Correlation of Solubilities of Organic Phosphorus Compounds
WANG Li-sheng,OUYANG Xia,HAN Jun,WU Jun-sheng
The synthesis and measurement of the solubilities of triphenylphosphine(TPP),tri-(4-methoxyphenyl) phosphine(TMOPP) and tri-(4-methoxyphenyl) phosphine oxide(TMOPPO) were introduced.The solubilities were correlated with temperature and an empirical equation of solubility was regressed.
2006 Vol. 23 (5): 420-422 [
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5363
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423
Prediction of Vapor-Liquid Equilibrium Using Modified UNIFAC Model Parameters Combined with the Mixing Rule of HVOS
WANG Xiao-qing,XUE Rong-shu,WEI Shun-an
The model for predicting vapor-liquid equilibria of mixtures at an infinite pressure reference state was presented by PR equation of state combined with Larsen UNIFAC activity coefficient model using the Orbey and Sandler's mixing rule of HVOS.In this model the parameter C~* in equation of state was given without the change of temperature,C~*=(-0.623 23).A revision of total 12 pairs of group interaction parameters of Larsen UNIFAC model was done by using the latest vapor-liquid equilibrium data in large range of temperature and wide range of systems.And predictions of vapor-liquid equilibria including alcohol,acid,ketone,water,nitrile and amine systems were made by using the new parameters and original parameters respectively.The results show that a significant improvement of prediction was achieved for many systems.The mean absolute deviations of calculation of vapor-composition were less than 4.00×10~(-2),and the mean relative deviations of bubble-pressure was less than 6.00%.
2006 Vol. 23 (5): 423-427 [
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2136
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428
Synthesis and Surface Activities of a Sulphonate Gemini Surfactant
YANG Yang~1,ZHENG Bao-jiang~1,YI Chang-chun~2,CHENG Fa~1
A sulphonate Gemini surfactant(Gemini-A) was synthesized from nonylphenol(NP)and formaldehyde and its structure was confirmed by elementary analysis and IR.Critical micelle concentration(cmc) and surface tension of Gemini-A were obtained from surface tension curves.They were 0.141 mmol/L and 33.51 mN/m respectively.The wettability of Gemini-A was studied by measuring the relative contact angle of the aqueous solution on the microscope glass slice.Solubilization of Gemini-A was investigated and compared with the traditional surfactants.Results showed that the aqueous solution of Gemini-A had high surface activities and high solubilization and it was a good surfactant for third times of oil extraction.
2006 Vol. 23 (5): 428-431 [
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3087
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2716
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432
Nickel-Sulfur Alloy Used as Water Electrolysis
LIU Yan-jie~1,SHAN Zhong-qiang~1,TIAN Jian-hua~1,WU Feng~2
Nickel-sulfur alloy based on nickel net was obtained by electro-deposition.On the given solution composition and electro-deposition current and temperature, the influence of the electro-deposition time on the hydrogen evolution reaction overpotentials of the Ni-S alloy was analyzed.The results of experiment showed that the hydrogen evolution reaction overpotentials of the Ni-S alloy reduced 130 mV compared with those of the cathode that wasn't electrodeposited.The Ni-S alloy performs an excellent electrocatalytic property for the hydrogen evolution reaction.
2006 Vol. 23 (5): 432-435 [
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1781
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2834
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436
Improving Hydraulic Surface Loading of Secondary Sedimentation Tank by Intermittent Sedimentation Process
LIU Yan-ping~1,ZHAO Lin~1,CUI Zhi-feng~2
To study the effect of the static settlement on the overflow rate,the simulating experiment was conducted on the traditional sediment tanks including the vertical-flow tank and the horizontal-flow tank which was run respectively under continuous settlement and intermittent settlement.Given the same quality of the influent and getting the same quality of the effluent,the result shows that the value of the overflow rate in the intermittent settlement process of the alternated internal-cyclic system(AICS) can be about 4 times higher than that in the continuous settlement process.This result will provide theoretical reference for choosing a higher value of the overflow rate in the designs of similar processes of AICS with a theoretical basis.And the application of this result will significantly reduce the investment of the project.
2006 Vol. 23 (5): 436-441 [
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1801
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442
Development and Application of Continuous Distillatian of p-tert-Butylphenol
PENG Yan-long,SUN Wei,JIA Shao-yi,WU Song-hai
A continuous distillation technique is exploited for production of p-tert-butylphenol by means of simulation and design of process by which the mixture of tert-butylphenol can be separated.Compared with traditional batch distillation technique,the application of the continuous distillation technique in industry showed that it has characteristics of high purity and yield of product,steady quality of product,low energy consumption.Applying the continuous distillation technique in the production of p-tert-butylphenol is reasonable, and has promising applications.
2006 Vol. 23 (5): 442-445 [
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2111
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181KB] (
2653
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446
Behavior of Bubbles in Non-Newtonian Fluids
FAN Wen-yuan,ZHU Chun-ying,MA You-guang,YU Guo-cong
Non-Newtonian fluid is widely encountered in many disciplinary fields,such as chemical engineering,foodstuff,biology and clinic,etc,and also closely related to many industrial processes and the life process of human being.The bubble behavior in non-Newtonian fluids directly affects mass transfer,heat transfer and the fast and slow of chemical process in fluids.Therefore,the understand and study of the bubble behavior in non-Newtonian fluids is of importance.In this paper, the research progresses of bubble behavior in non-Newtonian fluids are introduced and reviewed respectively from 3 aspects: formation,coalescence and collapse.
2006 Vol. 23 (5): 446-452 [
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4655
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453
Progress in Modification of Montmorillonites
ZHAO Bao-lin,NA Ping,LIU Jian-feng
Modified montmorillonites have been proved to be one of the most interesting mineral materials used in adsorption,catalysis and catalytic supports,photocatalysis and so on.The pillared montmorillonite interlayer is a special site in chemical reaction.The structure and elementary property of montmorillonite were introduced in this paper,and the modifying methods and mechanism were emphatically discussed.Advance in modification of montmorillonites,including inorganic modification,organic modification and inorgano-organo-modification was summarized.And the existing problems and applying prospect of modified montmorillonites were proposed.
2006 Vol. 23 (5): 453-457 [
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9000
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6852
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458
Progress in Non-Phosgene Synthesis of 4,4′-Diphenylmethane Diisocyanate
LI Fang,WANG Yan-ji,MIAO Jing,ZHAO Xin-qiang
The applications and production of 4,4′-diphenylmethane diisocyanate are described.Focus is laid on the discussion of the development of the non-phosgene methods by which 4,4′-diphenylmenthane diisocyanate is synthesized and the exiting problems.Synthesis of 4,4′-diphenylmenthane diisocyanate from dimethyl carbonate is proposed to have great potential.
2006 Vol. 23 (5): 458-462 [
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4508
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4103
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463
Recent Approach of Aqueous Two-Phase Extraction
XIE Hai
Aqueous two-phase extraction(ATPE)was growing up with the application of the continuous operation technique in the conventional equipment controlled by computer recently.The features of the traditional aqueous two-phase systems(ATPS)and the novel ATPS,the basic principles of the phase separation,and some shortcomings in application are summarized.It is proposed that the new development of ATPS is to find the suitable compositions which have low cost,easy reusability and high selectivity to the preseparated components.The thermodynamical models of ATPS liquid equilibria,the correlation method of the partition coefficient,and some unresolved problems of the ATPE are discussed.To improve the selectivity and the separating efficiency are key to the practical study of ATPE.To analysis the effects on partition coefficient and to revise the thermodynamical models of liquid equilibria are necessary to theoretical study of ATPE.
2006 Vol. 23 (5): 463-466 [
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2004
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467
Progress in Syntheses of Brassinosteroids and Related Compounds
SUN Shao-feng,ZHOU Xue-qin,LIU Dong-zhi,LI Lin
This paper reviewed the progress of structure-activity relationship and chemosynthetic methods of brassinosteroids in recent years.On the basis of analyzing structure-activity relationship,the key points and solving methods of synthesizing brassinosteroids are introduced from the synthesis of matrix-cycle and introducing side chain.
2006 Vol. 23 (5): 467-471 [
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1823
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