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Current Issue
2007 Vol.24 Issue.1,
Published 2007-01-15
Article
Article
1
Preparation and Performance of LiFePO_4/C Composites
TIAN Jian-hua~1,LI Xiang-jun~
LiFePO_4/C composites,as a kind of positive electrode materials in Li-ion batteries,were prepared by high temperature solid-state reactions.LiFePO_4 and LiFePO_4/C particles in the size from nanometer to sub-micrometer were obtained through pretreatment at 300 ℃ and calcination at 650 ℃.X-ray diffraction (XRD) analysis showed that the prepared LiFePO_4 and LiFePO_4/C composites had a structure of olive-type phase and with a high degree of purity.Among LiFePO_4 and LiFePO_4/C composites prepared with different carbon materials,such as the acetylene black,Vulcan XC-72 carbon black,scalelike graphite,anisotropic graphite powders and glucose,LiFePO_4/C samples prepared with glucose exhibited the best recharge-discharge cyclic performance.The cyclic performance was improved while the operation temperature was increased from room temperature to 40 ℃.This is because of the highe electronic conductivity and the more rapid diffusion rate of Li~+ in the LiFePO_4/C structure.
2007 Vol. 24 (1): 1-4 [
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4383
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5
Effect of Particle Size on Isobutene Hydration Reaction
YUAN Man,XU Chun-jian,ZHOU Ming,ZHANG Jun-mei
The effect of particle size on reaction rate of isobutene hydration was investigated in the slurry semibatch agitated reactor with fine powder of NKC-9 ion exchange resin.The results showed that when the particle size was above 105 μm,the internal diffusion resistance can not be neglected.When the particle size was below 30 μm,the reaction rate increased greatly with the decrease of partical size.
2007 Vol. 24 (1): 5-7 [
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3484
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3138
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8
Influence of Free Radicals on Catalytic Reduction of Sulfur Dioxide in the Presence of Oxygen over Sulfurized LaCoO_3
ZHAO Long,MA Zhi,QIN Yong-ning,QI Xiao-zhou
The influence of free radicals on catalytic reduction of sulfur dioxide by carbon monoxide in the presence of oxygen over sulfurized LaCoO_3 was discussed.It is found that oxygen poisoning can be eliminated through the reaction with free radicals produced by pyrolysis of acetone,thus the activity of the catalyst can be well maintained.XRD and XPS were used to investigate the influence of free radicals on the catalyst's bulk phase and surface state.
2007 Vol. 24 (1): 8-10 [
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2055
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249KB] (
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11
Influence of Phosphate Carrier Materials Belonging to NZP Family on the Activity of Vanadium Catalyst
ZHU Lin-hua,DUAN Feng-min
The vanadium catalysts supported by three different composition phosphate carriers belonging to NZP family were prepared by wet-blend method,and their active composition is the same as that of home-made S101 vanadium catalyst.The phase,specific surface area and pore structure of these catalysts were characterized by X-ray diffraction(XRD) and BET methods,and their activities were also evaluated in a small fitted-bed reactor.The results show that the chemical composition of the carriers has important influence on the activity of vanadium catalysts.KZr_2(PO_4)_3 is fit for being the candidate carrier of vanadium catalysts.
2007 Vol. 24 (1): 11-15 [
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1865
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349KB] (
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16
Synthesis of Cetyl Phthalate by Non-Acid Catalyst
PAN Zhao-qun,KANG Ying-zi,HUANG Kuo
Cetyl phthalate was prepared from phthalic anhydride and cetyl alcohol as raw materials catalyzed by non-acid catalyst.The effects of reaction temperature,reaction time,catalyst and the molar ratio of raw materials on the yield of product were discussed.The experimental results showed that the yield of cetyl phthalate was up to 98% when the reaction temperature was 220 ℃,the ratio of cetyl alcohol to phthalic anhydride was 3.0,the mass concentration of catalyst was 0.2%,the reaction time was 4.5 h,the adding temperature of catalyst was over 180 ℃.The whole process can be carried out under mild reaction condition,easy manipulation,post-treatment,short reaction time and without any waste gas, water or solid produced.The IR spectrogram of the product was identical with that of the target product.
2007 Vol. 24 (1): 16-19 [
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1045
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20
Composition and Performance of Spherical Superabsorbent Copolymer
XU Yong-shen,PAN Fan-fan,ZHU Li-ping,YUAN Cai-deng
The superabsorbent copolymers of partially neutralized acrylic acid(AA) and acrylamide(AM) were prepared by inverse suspension polymerization in the presence of crosslinking agent of N,N′-methylenebisacrylamide.The influence of monomer composition on copolymer composition,absorption characteristics and microsphere morphology was investigated.The reactivity ratio of AM was smaller than that of AA in the copolymerization so that the copolymer composition of microspheres was inhomogeneous in batch process.The water absorption capacity of crosslinked microspheres decreased with the increase of AM contents.But the absorptions of copolymer in salinity water exhibited synergic efficiency when the content of AM in monomer was 30%(mass ratio).The microsphere morphology of polymer of partially neutralized AA was spheric regularly,while that of the copolymer of AA and AM was spheric irregularly.
2007 Vol. 24 (1): 20-23 [
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1317
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24
Preparation of Paclitaxel-Loaded Polymeric Micelles by Dialysis Method
WANG Cai-xia,FENG Xia,XU Fang,LIN Bao-rui
Poly(ethylene glycol)(PEG)-conjugated linoleic acid(CLA)(PEG-CLA) polymeric conjugate was synthesized using 4-dimethylaminopyridine(DMAP) and dicyclohexycarbodiimide(DCC) as catalyst and coupling agent,respectively.PEG-CLA polymer was employed as carrier,the paclitaxel-loaded micelles were prepared by dialysis method.The size and size distribution,the structure and the surface chemistry of micelles were characterized by dynamic light scattering(DLS),transmission electron microscopy(TEM) and X-ray photoelectron spectroscopy(XPS),respectively.The in vitro release profiles of paclitaxel from polymeric micelles were investigated in pH7.4 phosphate buffer solution(PBS) and 1 mol/L sodium salicylate medium.The results show that the paclitaxel-loaded micelles have spherical shapes,particle size of 100 nm and narrow size distribution.XPS indicates that the drug is not absorbed on the micelles surface and sodium salicylate medium can accelerate the release rate of paclitaxel from polymeric micelles.
2007 Vol. 24 (1): 24-27 [
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1358
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28
Adsorbents for Removing Sulfur in High Sulfur-Containing Diesel
WU Zuo-xiang~1,HE Yan-jun~2,XU Dan-feng~1,LIU Bing-si~1
Desulfurization of high sulfur-containing diesel(mass fraction of(1 600)×10~(-6)) by different Cu~(2+) zeolites was analyzed in a fixed-bed adsorber.The zeolites were prepared by both direct synthesis and ion-exchange methods with HZSM5,then used for adsorption desulfurization of diesel fuel at room temperature and atmospheric pressure.The CuMCM41 adsorbent is capable of treating 5 mL of high sulfur-containing diesel fuel per gram of adsorbent,desulfurizing the diesel to concertrations less than 300×10~(-6)(mass fraction).These sorbents have been proven to have high sulfur-selective ability.CuMCM41 was used to adsorb model diesel,the results showed that CuMCM41 adsorbed more thiophenes and benzothiophene than naphthalene from model diesel.
2007 Vol. 24 (1): 28-31 [
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1266
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32
Process for the Synthesis of Salicylaldehyde by Esterification-Oxidation
WANG Yuan-bo,TIAN Song-jiang,LI Shu-fen
In this paper,investigation has been made on the process for the synthesis of salicylaldehyde by esterification-oxidation with phenol,paraformaldehyde(PF),boric acid as initial materials.Improvement was made on the esterification step,and depolymerization of PF in gas state was adopted as input manner in hydroxymethylation step.Meanwhile,reaction temperature in hydroxymethylation step,water content in PF,the amount of catalyst were discussed and the optimal operating conditions were attained under the optimal conditions.The yield of salicylaldehyde was 60.5% with purity of 98%.
2007 Vol. 24 (1): 32-35 [
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1062
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36
Coating Technology of Super-Weatherable TiO_2 Pigment
LI Wen-sheng~
Weatherability is one of important capabilities for TiO_2 pigment.The super-weatherability of TiO_2 pigment is obtained by a new fine SiO_2 coating preparation method.The effects such as adding method and adding amount of coating agent,temperature and pH,etc,on super-weatherability were analysed.The mechanism of fine SiO_2 coating was discussed and acid solubility was adopted to identify coating effect.The TiO_2 pigment with super-weatherability was produced under the condition that adding method is parallel-current,adding amound of coating agent is 3.5%,t=90 ℃,pH=9.5—10,Al_2O_3 is used as coating material.The result of anti-ageing experiment is above(6 000) h.
2007 Vol. 24 (1): 36-39 [
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1379
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40
Study on Polymerization Stability of St-BA-AA Copolymeric Latex
JIE Yu,ZHANG Yi-min,WANG Hong,ZHENG Bin,WANG Meng-yan
Styrene-butyl acrylate-acrylic acid latex had been prepared with the emulsion polymerization method by use of SDS,SDBS,OP-10 as the emulsifiers.The influence of temperature,the amount of initiator,the amount and the ratio of emulsifiers on the preparation process were discussed.It was found that the latex with lowest amount of coagulation was obtained,when the amount of initiator was 0.5%,the amount of emulsifiers was 4%,SDS∶SDBS∶OP-10 was 2∶1∶9,reaction temperature was 80 ℃±2 ℃ and the amount of acrylic acid was 2%.
2007 Vol. 24 (1): 40-43 [
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1243
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44
Improving Liquid-Solid Distribution Uniformity by Using Concentric Tube
WANG Yi-ping~1,WU Chen-xi~1,LIU Jun-jie~1,ZHU Li~2
Based on theories of branched pipe line and solid-liquid fluidization,a new type of combined distributor was developed for multi-pipe liquid-solid circulating fluidized bed.Distribution of solid particle in the pipe bundle was analysed in a cold model system and solid holdup and particle circulation rate were investigated.Experimental results show that the combined distributor,which is arranged in the inlet of chamber of the multi-pipe liquid-solid circulating fluidized bed,can effectively improve the uniformity of solid particle in the pipe bundle.
2007 Vol. 24 (1): 44-47 [
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1212
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48
Preparation of Tanshinones from Salvia Miltiorrhiza Bunge by HSCCC
QU Yi~1,YANG Yue-wu~2,GUO Zhi-xin~2,ZHU Guo-guang~2
Separation and preparation of tanshinones from Danshen(Salvia miltiorrhiza Bunge) crude ethanol extract were studied by high-speed counter-current chromatography(HSCCC).The solvent system of petroleum ether-ethyl acetate-methanol-water(8∶6∶7∶3) was selected and the optimum running parameters for apparatus was obtained through orthogonal experiment.Five tanshinone were separated and identified rapidly.Measured by HPLC,the purity of tanshinone ⅡA,cryptotanshinone,tanshinone Ⅰ,dihydrotanshinone Ⅰ were all over 98%.HSCCC is simple,economical,quick and with good repeatability for preparation of Danshen active components.
2007 Vol. 24 (1): 48-51 [
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1133
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52
Application of Gas Sparging to the Production Process of Xylose by Ultrafiltration
JI Wei,LI Shi-zhong
In the current industry,the xylose is manufactured by corncobs through hydrolysis,neutralization,twice decoloring with activated carbon,twice ion-exchange treatments and some other steps.But the process is costly and complex.In this paper,ultrafiltration was introduced into the production process of xylose.The effect on ultrafiltration treatment was analyzed,such as trans-membrane pressure,fluid flux,and temperature.The result showed the ultrafiltration treatment can cut down impurity and purify the xylose solution.In the ultrafiltration, gas sparging was used to deal with the tricky problems such as concentration polarization and membrane fouling.Lots of tests proved ultrafiltration can replace one decoloring with activated carbon,simplify the process,and can be applied to the production of xylose.
2007 Vol. 24 (1): 52-55 [
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1410
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56
Comparisons of Pressure Drop and Separation Performance Between Two Rotating-Stream Tray Separators
SUN Wen-shou~1,WANG Gao-sheng~2
The pressure drop and separation efficiencies were measured and analyzed in a 300 mm single-path rotating-stream tray(RST) separator and a double-path RST separator.The pressure drop of the double-path RST separator decreased by 12.8% of that of the single-path RST separator.For the double-path RST separator,the workable gas velocity range was greatly increased,and no significant effects of gas velocity and spray density on separation efficiency and entrainment were observed,and the separation efficiencies were above 99.9% within the experimental range.When the tray vane exit velocity varied from 10 m/s to 17 m/s,the amount of mist escaped from the double-path RST separator decreased by 72.7% to 96.3% of that from the single-path RST separator.The advantages of double-path RST separator over single-path RST separator are the integrated effects of increased tangential velocity,elimination of the vortex rings in most axial plane region,and the decreased separation distance.
2007 Vol. 24 (1): 56-59 [
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2213
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60
Experimental Study on Small-Scale PSA Oxygen Generating
BU Ling-bing,LIU Ying-shu,ZHANG De-xin,LIU Wen-hai
The effects of some main factors,such as the species of molecular sieve,exchange time,pressure equalization process,ratio of height to diameter,the volume of tank on the process of small-scale pressure swing adsorption(PSA) oxygen generating are discussed experimentally.The experimental results show that different species of molecular sieve have different productivity and LiX is best;using LiX molecular sieve can decrease the volume of oxygen concentrator and improve the characteristics;with the increase of exchange time,the oxygen purity increases in the beginning and then decreases,the optimal exchange time is defined by experiment.The pressure equalization may improve the oxygen purity and recovery,the oxygen purity and recovery of the pressure equalization process in absorber's two-lets are the biggest.Increasing the ratio of height to diameter of the absorber can improve the oxygen purity,but it is not good if the ratio is too big.Increasing the volume of tank can also improve the oxygen purity.
2007 Vol. 24 (1): 60-64 [
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1476
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65
New Technique for Recovery of the Used Catalyst by Soaking in Complex Acid
HAO Xi-cai~1,WANG Fang-lin~2,HU Bin-jie~2
As an important chemical,methanol's production is increasing,it is urgent and important to research on the recovery of the used catalyst.A new process which produce copper sulfate pentahydrate and activated zinc oxide from the used catalyst by soaking in complex acid has been introduced in this paper.The process is simple and the product has high additional value,the quality reaches to GB437-80 and GB/T3185-92.The value in economy and in society is great.A new path is proposed to recover the used catalyst in the preparation of methanol and to eliminate environmental pollution.
2007 Vol. 24 (1): 65-68 [
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1079
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69
Supercritical Fluid Technique for Preparing Fine Particles and Its Application in Catalysts
ZHAO Shu-fang,LIU Zong-zhang,ZHANG Min-hua
The use of supercritical fluids(SF) as media for the preparation of fine particles is developed recently.This paper describes two routes to particle formation: the rapid expansion of supercritical solution and the supercritical antisolvent(SAS).Based on SAS,some improved SF technologies in preparing microparticles,such as ASES,SEDS and SAS-EM are introduced briefly.In addition,the influences of technical conditions on the particles size and size distribution are introduced.Emphasis is put on the application of supercritical fluid technique for preparing microparticles in catalysts.Finally,the main problem and prospect are proposed.
2007 Vol. 24 (1): 69-74 [
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1338
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75
Progress in Hydrodynamics and Mass Transfer in Bubble Column Reactor
HE Guang-xiang,YANG Suo-he,JIN Hai-bo
The flow behavior,axial liquid mixing and inter-phase mass transfer in bubble column reactor were reviewed.The measurement methods of gas holdup,liquid velocity,axial liquid dispersion coefficient and volumetric mass transfer coefficient were introduced.And the difference among different methods was introduced.Effects of system pressure,temperature,superficial gas velocity,liquid properties and solid holdup on the flow behavior,axial liquid mixing and mass transfer in bubble column reactor were discussed.
2007 Vol. 24 (1): 75-80 [
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1358
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317KB] (
3462
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81
Progress in Synthesis of Terephthalic Acid
HAN Jin-yu,DONG Yang,FANG Jian,WEI Wen-ying,MAO Wei
In this paper,the methods and processes of producing terephthalic acid(PTA) were introduced,especially the technology,catalyst and reaction conditions of supercritical water oxidation.The advantages and disadvantages of several major technologies were summarized.And the prospect of the PTA technology was proposed accordingly.
2007 Vol. 24 (1): 81-85 [
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1228
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278KB] (
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86
Review on Process for Purifying Nitrogen Trifluoride
PENG Li-pei,WANG Shao-bo,LI Shao-bo,FU Man
This paper reviews the basic physical and chemical property of nitrogen trifluoride,including its production method.In order to meet the need of semiconductor industry,the applied purification methods for nitrogen trifluoride are:cryogenic distillation,azeotropic distillation,absorption,selective adsorption and the combination of them.
2007 Vol. 24 (1): 86-90 [
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1722
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Production of Organic Fertilizer Fixing Sand and Maintaining Soil from Waste Liquid of Papermaking
HE Min~1,HUANG Jun-fa~2,HE Xiu-yuan~2
Environmental organic fertilizer which can fix sand and maintain soil was obtained by environmental black liquor produced in papermaking process after evaporation,improved treatment.The black liquor contained large amount of lignin with great cohesive property because soda was replaced by magnesium ammonium in the papermaking process.The experiments in room and out room were carried out in China Academic Sinica Desert Laboratory.The results indicated that:the effect of fixing sand is obvious,the anti-wind erosion performance is very good.Because the organic content is nearly 40%,it can give nutrient for desert and sand,and favor the desert plant to grow to obtain long-term fixing sand.To widely apply this complete set of innovation technology can not only eradicate the pollution of waste liquid of papermaking but also solve the technical difficult problem on fixing sand and controlling desert.It has notable benefit in environment,society and economy.
2007 Vol. 24 (1): 91-94 [
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1055
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2007 Vol. 24 (1): 95-95 [
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754
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