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2007 Vol.24 Issue.5,
Published 2007-09-15
Article
Article
374
2007 Vol. 24 (5): 374-374 [
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Hydrodynamics of Air-Catalysts of SRNA-4 in Magnetically Stabilized Bed
ZHANG Jin-li~1,WU Yue-jiang~1,MENG Xiang-kun~2,ZONG Bao-ning~2
Pressure drop,minimum fluidized velocity,solid holdup,local solid holdup distribution and gas phase backmixing are fundamental to the scale-up design and optimization of gas-solid(G-S) magnetically stabilized reactors.In this article,the hydrodynamics were studied using the pressure drop method,the photoelectric method and the transient point source tracer pulse input technique for the G-S magnetically stabilized bed taking the ferromagnetic amorphous alloy catalysts of SRNA-4 as the solid phase.The minimum fluidized velocity and the related bed voidage were observed to be independent of the magnetic field.The radical distribution of the solid holdup was uniform,and the local solid holdup increased owing to the inhibition of the particle movement by the magnetic field.However,increasing the superfacial gas velocity can promote the expansion of the GS bed,and decrease the solid holdup.For small particles,Pe number did not change greatly as the magnetic field and gas velocity changed,while for large particles Pe number decreased as the magnetic field increased,and the increase of magnetic field made the Pe number increased at the beginning then followed by decreasing.Based on the experimental data,the correlated equation was obtained to estimate accurately the minimum fluidized velocity,solid holdup and bed height.
2007 Vol. 24 (5): 377-380 [
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381
Synthesis of 2,4,6-Trimethylbenzaldehyde
WANG Fei~1,ZHANG Xiao-xing~1,FENG Rong-xiu~2,SONG Jian~2
2,4,6-trimethylbenzaldehyde was synthesized through Gattermann-Koch reaction,and the reaction condition was optimized.The effects of reaction temperature,pressure of carbon monoxide,the amount of hydrochloric acid,and the promoter were discussed.The reaction can be promoted by titanium(Ⅳ) chloride(TiCl_4) and ethyl ether.The optimized condition is:the molar ratio of 2,4,6-trimethylbenzaldehyde to anhydros aluminum chloride(AlCl_3) is 3.08,molar ratio of AlCl_3 to concentrated aqueous hydrochloride is 550,weight ratio of anhydros AlCl_3 to TiCl_4 is 45,pressure of carbon monoxide is 1.06—1.48 MPa,at 26—(28 ℃),for 20 h,yield of 86.86%.
2007 Vol. 24 (5): 381-384 [
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1916
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385
Preparation of Pd/HZSM-5 Film Catalyst for Cracking of n-Dodecane
MENG Fan-xu,ZHAO Hai-long,ZHANG Xiang-wen,LI Jia,ZOU Ji-jun
A method for the preparation of Pd-supported HZSM-5 zeolite film was described.The cracking of jet fuel model compound of n-dodecane in Pd/HZSM-5 catalyst-coated tube was studied.The Pd/HZSM-5 film was characterized by SEM and XPS.It was shown that,the surface was approximately flat and the thickness of the zeolite-coating layer was about 10 μm.And Pd existed as metallic state.The heat sink and the decomposition under 4 MPa at(600 ℃,) showed that the heat sink could be enhanced due to the existence of zeolite HZSM-5,and Pd/HZSM-5 film can increase the heat sink by 16.9%.
2007 Vol. 24 (5): 385-388 [
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389
Hydrogen Production by Ethanol Steam Reforming over Pd/γ-Al_2O_3 Catalyst
WANG Hao,ZHANG Yue,MA Xin-bin
The reaction of ethanol steam reforming for hydrogen-rich gas streams production,over a commercial alumina supported palladium catalyst was investigated.In particular,the dependence of the catalytic activity and selectivity on reaction temperature,Pd loading with γ-Al_2O_3 was studied.In order to evaluate the catalytic stability,long-term experiments were also performed.Hydrogen selectivity was proportional to the high Pd loading or high reactor temperature.Hydrogen selectivity up to maximum value(136%) were obtained at 5%Pd/Al_2O_3(weight ratio)under(650 ℃) reactor temperature.And hydrogen selectivity up to 110% was obtained at temperature close to(750 ℃) with 1%Pd/Al_2O_3(weight ratio)catalyst.Pd/Al_2O_3 catalysts was characterized using NH_3-TPD,TGA.
2007 Vol. 24 (5): 389-393 [
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394
Synthesis and Characterization of Cellulose-Based Polymeric Surfactant
WEI Yu-ping,HOU Gui-li,CHENG Fa
Cellulose-based polymeric surfactant was synthesized by two steps using cellulose with DP of 280 as raw material.Microstructure and properties were investigated by Fourier transform infrared spectroscopy(FTIR),dynamic contact angle analyzer,transmission electron microscopy(TEM),dynamic laser scattering(DLS) analysis.Results showed that critical aggregate concentration(CAC) of this amphiphilic polymer was 0.60%(weight of percent)and corresponding surface tension was 57 mN/m.TEM and DLS results demonstrated that micelles in aqueous solution spontaneously aggregated near CAC.When the concentration increased from 0.5% to 1.0%,the particle size increased also from 388.0 nm to 549.7 nm.In addition,the rheological behavior of this polymer was similar to conventional synthetic polymer.
2007 Vol. 24 (5): 394-397 [
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398
Crystallization and Separation of L-Arabinose from Hydrolysate of Arabic Gum
GUO Jun-wei,FENG Ya-qing,WANG Jing,LIU Da-wei
Crude L-arabinose was prepared from arabic gum hydrolysized solution by crystallization.The effects of time,temperature,pH value and solvent on the yield and purity of L-arabinose were discussed.The technical conditions of the crystallization and separation process of L-arabinose from the hydrolysate arabic gum were obtained.This simple method was efficient and easy for industrial production.
2007 Vol. 24 (5): 398-400 [
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401
Synthesis of 3-Carbonyl-Androsterone-4-Alkene-17β-Acid
LUO Jin-feng,ZHOU Xue-qin,LIU Dong-zhi,YANG Xiong-wen
Important steroid intermediate 3-carbonyl-androsterone-4-alkene-17β-acid was synthesized from DHEA by Wittig reaction,hydroboration-oxidation,Oppenauer oxidation and Jone's oxidation in total yield of 23.0%.The structures of products were identified by NMR,MS and IR.
2007 Vol. 24 (5): 401-403 [
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404
Improved Synthesis of 2-Allyl-4-Hydroxy-2-Cyclopentenone
SHAO Huai-qi~
2-allyl-4-hydroxy-2-cyclopentenone,a key synthetic intermediate for the synthesis of prostaglandins of 4-thia-PGI_1,is of important biological activity.2-allyl-4-hydroxy-2-cyclopentenone was synthesized from furfural by an improved method through Grignard reaction and rearrangement reaction.The effects of the acid catalyst,solvent,acid concentration and reactive temperature on the rearrangement were investigated.The results showed that polyphosphoric acid has better catalytic aceivity,the yield of the rearrangement is 79% and purity is 99.2% at 100 ℃ when molar rate of polyphosphoric acid to raw material is 0.2.The total yield is 64%.
2007 Vol. 24 (5): 404-407 [
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408
Separation of Benzoic Acid Residua by Vacuum Distillation
LI Shu-yi,WEI Feng,YANG Tao,HAN Li-guo
The fraction of benzyl benzoate and fluorenone were enriched from benzoic acid residua by flash distillation,then separated by vacuum batch distillation,so the recovery of benzoic acid residua was implemented.The experiment showed that this separation method is feasible and benzyl benzoate with purity about 90% and fluorenone products with purity of more than 85% were obtained.Furthermore the effects of tower top pressure,temperatures of tower top and bottom,reflux ratio on product purity were analyzed.The optimal operating condition was determined in the experimental condition.
2007 Vol. 24 (5): 408-411 [
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412
Preparation and Characterization of Kaolinite/Tartaric Acid Intercalated Compound
ZHAO Shun-ping,WANG Xu-fan
Kaolinite/tartaric acid(K/T)intercalated compound was prepared by replacing method of dimethyl sulphoxide(DMSO).The product was characterized by XRD-6000 and FTIR.The XRD showed that the basal spacing of kaolinite increased from 0.72 nm to 1.09 nm,and the apparent intercalation of product was 50%.The FTIR spectrum indicated that hydrogen bonds were formed between the carbonyl group in tartaric acid and the hydroxyl group in inner surface of kaolinite.Hydrogen bonds can also be formed between the hydroxyl group in tartaric acid and the oxygen atom of silicon and the oxygen layer in kaolinite.The tartaric acid molecule was tiled between kaolinite layers with single molecule layer.
2007 Vol. 24 (5): 412-415 [
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416
Synthesis of NH_3 by Radio-Frequency Discharge
WANG Yu-ping,TAN Shi-yu,YAO Fang-hua
NH_3 was synthesized from N_2 and H_2 under low pressure(≤0.1 MPa) by radio-frequency discharge at 13.56 MHz.The effects of configuration of reactors, discharge voltage,discharge area,ratio of N_2/H_2 and flux of total gas on the synthetic reaction were studied.The volume fraction of NH_3 can reach 1.2% under the optimal condition.
2007 Vol. 24 (5): 416-419 [
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420
Separation Process of Sodium Chloride from Synthesized Betaine by Extraction Crystallization
WANG Shuang-ping~1,JIN Deng-chao~2,HU Jun-feng~3,WANG Fu-min~1
Extraction crystallization,a new method for the separation of sodium chloride in betaine synthesis process,was introduced.Methanol was selected as the extractant to make the sodium chloride separate out to improve the purity of betaine.The results of the phase diagram and experiments indicated that after the disposal of ordinary distillation,the more the composition approached the saturated composition(m(betaine)∶m(sodium chloride)∶m(water)=3∶1∶1),the more sodium chloride was separated out.Furthermore,when the dosage of methanol was 75.3% in total,the crystal amount of the sodium chloride reached the most.
2007 Vol. 24 (5): 420-423 [
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1883
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424
Preparation of W-Catalyst Supported on Montmorillonite
WANG Wei,LIU Ji-chun,ZHANG Yu-qing,LUO Jie
WCl_6/t-BuArOH complex compound was prepared,which makes WCl_6 dissolved well in organic solvent and more stable in air.Through exchange with ions or groups in the interlayer of montmorillonite(MMT),WCl_6/t-BuArOH complex compound can form an intercalative complex catalyst.Results from XRD,SEM and TEM indicated that organically modified MMT can act as a good carrier for the WCl_6/t-BuArOH complex compound,whereas the nonmodified inorganic MMT can not.
2007 Vol. 24 (5): 424-427 [
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428
Technology of Manufacturing Nano-Sized Magnesium Hydroxide from Concentrated Seawater After Desalination
MA Jing-huan,ZHOU Jun,SUN Bao-hong,CHANG Fu-rong
High pure nano-sized magnesium hydroxide was prepared from concentrated seawater with seawater reverse osmosis desalination(SWRO) through a series of process, such as calcium eliminating,precipitating,washing with ceramic membrane,centrifugal filtrating and vacuum drying,etc.Experiment showed that the quality of magnesium hydroxide obtained by this process was better than chemical industrial standard(magnesia content is 67.9%,calcium oxide content is 0.2%) and the average grain diameter was below 100 nm.Washing and separating nano-sized magnesium hydroxide with ceramic membrane was feasible.The membrane equipment worked steadily and the average flux of membrane was more than 331 L/(m~2·h),the rejection rate of magnesium hydroxide was more than 99%.
2007 Vol. 24 (5): 428-432 [
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1934
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8
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433
Progress of Catalysts for Isobutylene to Methacrolein
LI Qiang~
Selective oxidation of isobutylene to methacrolein is a key step in the production of methyl methacrylate from isobutylene.The progress of catalysts,which include composite-oxides catalysts and heteropoly compounds catalysts,for selective oxidation of isobutylene to methacrolein were summarized,the mechanism of this reaction on Mo-Bi catalysts was discussed.
2007 Vol. 24 (5): 433-438 [
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439
Progress in Intensification of Nano-TiO_2 Photocatalytic Degradation
CHEN Wen-dong,WANG Chang,JIA Qing-zhu,LI Gui-ju
Based on photocatalytic technology,the development and characteristics of nano-TiO_2 photocatalytic materials are summarized.The principle of nano-TiO_2 photocatalytic degradation and the new technology of improvement on photocatalytic efficiency of nano-TiO_2 photocatalyst in present are introduced.The problem in practical application as well as advances in lab study have also been put forward.At the same time,some advice and solution ways are brought forward.The application and development on oxygenation technology in future are prospected.
2007 Vol. 24 (5): 439-445 [
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446
Progress in Synthesis and Functionalization of 7-Substituted Indole Catalyzed by Palladium
BI Wei-jia,LI Xiao-jun,ZHANG Guo-liang,ZHANG Feng-bao
7-substituted indole is key intermediates for forming synthetic drugs and fine chemicals.In this paper,the progresses in preparation methods of 7-substituted indole through palladium-catalyzed reactions in recent 15 years were reviewed.These methods are divided into two categories: the direct synthesis from substituted benzenoid derivatives and the functionalization of performed indoles ring,both of which are introduced in detail in the aspects of mechanism and the processes of reactions.
2007 Vol. 24 (5): 446-452 [
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453
Applications of Shape Memory Polyurethane
SONG Fei,ZHU Guang-ming,DENG Deng
The latest progress in shape memory polyurethane was summarized.The structures and characteristics as well as the applications of shape memory polyurethane were reviewed.The applications in the field of waterproof breathable fabrics were analyzed and the prospect in future was proposed.
2007 Vol. 24 (5): 453-456 [
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457
Progress in Computer-Aided Molecular Design Based on Group Contribution Method
SHENG Wei-xin,RONG Zong-ming,YING Xu-gen
Group contribution method can be used not only to estimate the properties of compounds,but also in computer-aided molecular design(CAMD).The principle of the CAMD based on group contribution method and its applications in solvents and polymers design were described in detail.And the methodology used in CAMD was also introduced.With the increase of the demand for green solvents and new polymers,the CAMD based on group contribution method will apply widely in these fields.
2007 Vol. 24 (5): 457-465 [
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466
Simulated Calculation of Primary Reformer of Branu Synthetic Ammonia Plant
HE Dong,WEI Shun-an
The heat transfer model of heart combustion and reaction kinetics model of gassolid catalytic reaction in tube are establish to simulate the process of radiant section of primary reformer of Branu synthetic ammonia plant.Hottle zone method is used to established three-dimensional radiative heat transfer model in heart combustion and it is combined with the reaction kinetics model of gas-solid catalytic reaction to calculate three-dimensional temperature distribution of hearth and the distribution of temperature,pressure and composition in tube.The simulation results are coincident with true value.Compared with conventional method,three-dimensional model used in the heat transfer process of hearth makes the results more accurate.The method and results are beneficial to energy saving,consumption reducing and equipment improvement.
2007 Vol. 24 (5): 466-471 [
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