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2008 Vol.25 Issue.3,
Published 2008-05-15
Article
Article
189
Correlation of the Cholesterol Solubilities in High-Pressure Carbon Dioxide with Association Model of Four Parameters
LIU Bo,WEN Zhen,ZHENG Zong-kun,YOU Xin-kui,PU Yi-tao
The solubilities of cholesterol in high-pressure carbon dioxide were determined by a dynamic method under 10 MPa—30 MPa at 313 K—343 K.It was found that solubilities of cholesterol were from 1.0×10~(-6) to 1.0×10~(-4).Based on the principle of solvation reaction and the equilibrium constant affected by pressure and temperature,Chrastil model was modified and an association model of four parameters was established.Then the experimental solubility data were correlated by the association model.The results showed there was a good agreement between experimental data and calculational data of the solubilities of cholesterol in high-pressure carbon dioxide.
2008 Vol. 25 (3): 189-193 [
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194
Preparation of SnO_2-Sb_2O_3-TiO_2 Conductive Powder and Its Electrical Conductive Coating
NI Yue-qin,XU De-shun,ZHANG Yi,LI Xiang-gao
The composite conductive powder with titanium dioxide powder covered by SnO_2 and Sb_2O_3 was prepared by chemical coprecipitation technology.The orthographic tests showed that the optimal preparation condition is m(TiO_2)∶m(SnCl_4)∶m(SbCl_3)=25∶15∶1,pH=1.5,hydrolysis temperature is 60 ℃ and calcinations temperature of the coprecipitation product is 700 ℃,the volumetric electrical resistivity of the powder is 77 Ω·cm with size below 200 nm.Conductive coating was then prepared on aluminum alloy substrate with phenolic resin as binder.The volume resistivity of the conductive coating could be below 10~8 Ω·cm,meanwhile the surface of the conductive coating was smooth without defect.
2008 Vol. 25 (3): 194-198 [
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199
Application of Micro-Displacement Method in Total Material Mass Measurement
WANG Yi-ping~1,HAO Peng-yue~1,LI Ke-jian~2,HUANG Qun-wu~1
In order to solve the measurement problem of total material mass in certain chemical processes,a novel method with the help of micro-displacement test was proposed based on the linear relationship of load and deformation.A suspension system which was used for supporting bubble column was taken as an example.The Finite Element Analysis and experiment method were applied respectively to validate the veracity of the micro-displacement method.And the results show that this measurement method is feasible.
2008 Vol. 25 (3): 199-202 [
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1658
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203
Hydrolysis of Propyl Trimethoxy Silane
LI Fang-wen~
In the paper,the hydrolysis of propyl trimethoxy silane(assigned with WD-10)was analyzed by the one-factor experimental method, conductivity detection and FTIR spectroscopy,and then the factors of affecting hydrolysis was discussed,the better technical parameters of hydrolysis were determined.The better technical parameters of hydrolysis are as follows: volumetric ratio of WD-10,secondary distilled water and methanol is 1∶1∶3;pH is 4;hydrolysis is at 30 ℃ for 4 h. This can provide reference for the oleophilic modification of porous ceramics filtering ball and the treatment of wastewater containing oil by coalescence filtration technique.
2008 Vol. 25 (3): 203-207 [
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2312
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208
Interaction of Rhodamine B with Micelles of Sodium Dodecyl Sulfate
LIU Jin-yan,LIU Cui-cui,GUO Gui-bao,WANG Zheng-de
Interaction of Rhodamine B(RhB) with micelles of sodium dodecyl sulfate(SDS) and the effect of mineral salt were analyzed by fluorescence spectroscopy.The results showed that RhB could be used as probe to determine the critical micellar concentration of surfactant SDS in aqueous solution.The intercation of RhB with micelle could be represented quantitatively by the association constant K_a.In the system,K_a increased with the increase of concentration of mineral salt,which showed that the interaction of RhB with SDS micelle increased.
2008 Vol. 25 (3): 208-211 [
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212
Clean Synthesis of Magnesium Stearate by Direct Method in Aqueous Medium
WU Mao-ying,LUO Yong-xin
By a specific process,high quality magnesium stearate with good color and luster was cleanly synthesized by the direct reaction of basic magnesium carbanate with stearic acid in aqueous medium under atmospheric pressure without any additive.It was shown that the rate of the synthetic reaction was affected obviously by the reaction temperature and liquid-solid ratio of the feed,and the first rate product of magnesium stearate could be synthesized under the following conditions:reaction temperature is 80 ℃,liquid-solid ratio of the feed is 6∶1,and reaction time is 300 min.Compared with that of traditional technology of double decomposition method,the productivity of this technology was raised and the consumption of energy and water reduced greatly.Since this process can make use of the production equipment in the double decomposition process,it can be adopted by the existing enterprises that originally using the double decomposition process to produce magnesium stearate to restructure in an environmentally friendly way.
2008 Vol. 25 (3): 212-214 [
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215
Preparation of Chitosan-Gelatin Drug Loading Microshpere and Its Release Characteristics
YAO Fang-lian,YU Xiao,ZHOU Yu-tao
A chitosan-gelatin drug-loaded microsphere with controlled release characteristic was prepared from chitosan and gelatin by emulsion coagulation method.Microspheres loaded with different quantity of drug were prepared via acetone marination-room temperature dried method and HCl marination-NaOH regeneration-freeze-dried method using isoquinoline as model drug,and then drug encapsulation and release behavior were studied.When the ratio of glutaraldehyde to chitosan was between 0.40 and 0.53 and drug loaded quantity was 20%—30%(mass ratio),nearly 75% drug was released during the first 15 h,and the ratio of drug encapsulation kept 40%—50%.The results provided foundational data for the application of chitosan-gelatin drug-loaded microsphere in biomedical field.
2008 Vol. 25 (3): 215-219 [
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Reduction of CaCO_3 Scale Formation During Pool Boiling by Sputtering MgF_2 on Surface
WANG Yan~1,LIU Ming-yan~1,WANG Ze-zhen~2,WANG Lin-lin~1,LIANG Wen-cai~1
The accumulation of unwanted crystalline deposits(fouling) reduced the efficiency of heat exchanger considerably.In this investigation,MgF_2 composite thin film was deposited on Cu substrate by magnetron sputtering.The fouling process of CaCO_3 in pool-boiling systems was performed.Scanning electron microscopy(SEM) was employed to determine the morphology of the substrate and surface energy was calculated.The experiment results showed that the sputtered MgF_2 surface reduced CaCO_3 deposit on the heat transfer surface significantly.
2008 Vol. 25 (3): 220-223 [
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224
Isopropylation of Naphthalene Catalyzed by Fe_2(SO_4)_3/Bentonite Solid Acid Catalyst
LI Ke-jing~1,JIN Hai-bo~1,ZHAO Zhen~2
Fe_2(SO_4)_3/bentonite solid acid catalyst was prepared by the bentonite disposed with H_2SO_4,and then dipped with Fe_2(SO_4)_3 solution.Isopropylation reaction conditions of naphthalene catalyzed by the(Fe_2(SO_4)_3/)bentonite catalyst were investigated using orthogonal design experiment method.The experimental results showed the optimum reaction condition is n(naphthalene)/n(isopropyl alcohol)=8,n(naphthalene)/n(decahydronaphtyalene)=7.5,reaction temperature is 260 ℃,reaction time is 6 h,m(catalyst)/m(naphthalene)=0.125.Meanwhile,the effect factors of isopropylation reaction of naphthalene were analyzed systematically.Furthermore,the Fe_2(SO_4)_3/bentonite catalyst was characterized for sour intensity,sour amounts and sour type using NH3-TPD and FT-IR methods.
2008 Vol. 25 (3): 224-228 [
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1960
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229
Facile Synthesis and Chiral Separation of β-Amino Acid Racemates
CHEN Feng,CHEN Lei
Optically pure β-amino acids are important components of natural products and essential intermediates of polypeptide and β-lactam.Traditional preparation methods involved multi-step synthesis,expensive raw materials,complicated operating procedures and low yields.In this paper,a novel approach to get β-amino acid enantiomers was described.With aldehyde,malonic acid,ammonium acetate as raw materials,five β-amino acid racemates were synthesized by one-pot method.These amino acids were then resolved by ligand exchange chromatorgraphy(LEC) to yield optically pure β-amino acids.The results showed that one-pot synthesis of β-amino acids and chiral separation by LEC was a simple and efficient method,by which the amino acid enantiomers can be produced with low cost and high yield.This method can be adopted for the preparation of β-amino acid enantiomers with different structures used in the high throughput screening of drug candidates during the process of drug development.
2008 Vol. 25 (3): 229-232 [
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233
Synthesis of Norgestimate
KANG Song~1,ZHOU Zi-qing~1,GAO Rui-chang~2
As a new generation of progesterone product,norgestimate is widely used as an oral contraceptive,acne therapy,and hormone replacement therapy for menopausal symptoms in women.In this paper norgestimate was obtained from levonorgestrel through di-esterization,acid hydrolysis and oximization reactions. UV,IR,H-NMR,C-NMR and Mass were performed to determine the structure of intermediates and final product.Results showed the analytical sample was identical to authentic,and the chemical structure and the quality of this compound agreed with those of imported samples.
2008 Vol. 25 (3): 233-236 [
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237
Michael Addition Catalyzed by a New Effective Catalyst of Y(OTf)_3
GAO Chang-shui~
The Michael addition of indoles or furan with α,β-unsaturated ketones catalyzed by Y(OTf)_3 was proposed to synthesize the corresponding derivatives.This method was easy to operate under mild conditions and with high yield.The catalyst Y(OTf)_3 was reuseable and was considered as environmentally friendly catalyst.
2008 Vol. 25 (3): 237-241 [
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1944
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242
Purification by Eichhornia crassipe in Ecological Watercourse
ZHU Hong-jun
The purification by Eichhornia crassipe in ecological watercourse was examined in indoor laboratory.Circles in three different forms were used to enclose the Eichhornia crassipe.Water purifying efficiencies of Eichhornia crassipe were analyzed in different conditions.The results indicated that the water purifying efficiency Eichhornia crassipe was great and it was a viable hydrophyte in ecological watercourse,but the nutrition should be considered.If the nutrition was not enough for water hyacinth's absorption,the Eichhornis crassipe would perish after some days.From the analysis of hydrodynamics,when the frames were disposed and Eichhornia crassipe were planted in channel,flow in this channel was influenced.Model C had the most influence on flow's configuration.Model A and B had a little affection,which were suitable for water purifying.
2008 Vol. 25 (3): 242-247 [
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248
Treatment of High Content Aniline Wastewater by Extraction
JIANG Xiao-yun~1,CHEN Song~2,LI Guo-bing~2
By comparing of several kinds of method for treatment of aniline wastewater,an extracting method using methylbenzene as extracting agent was proposed for the treatment of 40 g/L aniline wastewater produced in the manufacture of rubber antioxidant(RD).Based on the technological parameters obtained from experiment,a production facility whose capacity was 20 m~3/d was designed.The production showed that 98.5% of aniline was recovered.Compared with other means,the proposed extraction method has advantages such as less equipment investment,easier operation and lower consumption.
2008 Vol. 25 (3): 248-250 [
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251
Enantioselective Synthesis of Fluoxetine Hydrochloride
CAO He,LI Ai-jun,ZHOU Xue-qin,LIU Dong-zhi
Fluoxetine hydrochloride is a potent and highly selective inhibitor of neutral serotonin-reuptake and is one of the most important drugs for the treatment of psychiatric disorders and metabolic problems.Due to its market value and the different pharmacological activities displayed by analogues of fluoxetine, several synthetic methods,including the enantioselective synthesis of both enantiomers,have been reported.Progress in enantioselective synthetic methods of fluoxetine hydrochloride were reviewed in this paper.
2008 Vol. 25 (3): 251-258 [
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1943
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259
Progress in p-Dioxanone and Poly (p-dioxanone)
XU Xiang-kui,FENG Ya-kai,XUE Yan
Poly(p-dioxanone)(PPDO),one kind of aliphatic polyesters,has excellent biodegradability,bioabsorbability and biocompatibility,and also has good flexibility due to the unique ester bonds in polymer chains.So PPDO is used as films, molded products,laminates,foams,nonwoven materials,adhesives,and coatings. In this paper the progress in the synthesis,structure,property and application of p-dioxanone and poly(p-dioxanone) were reviewed.
2008 Vol. 25 (3): 259-263 [
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2524
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264
Progresses in Comprehensive Treatment of Nitrobenzene Wastewater
DONG Jian
Due to its high toxicity and refractory,nitrobenzene accumulated chronically were harmful to human beings.Pollution problems involved are being seriously concerned.The principal treatment processes for nitrobenzene wastewater are physical,chemical and biological processes.In this paper,the progresses in these three kinds of treatment technologies were reviewed.The emphasis and direction of the study in the future were prospected.
2008 Vol. 25 (3): 264-270 [
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271
Preparing 2-Fluoring-5-Nitroaniline by Reduction of Zinc Powder
WANG Qian,QIN Hai-fang
In this paper,2-fluorin-5-nitroaniline was prepared by reduction of 2,4-dinitrofluorin benzene catalyzed by zinc powder in the mixed solvent of ethanol/water.The optimum conditions were as follows: when mol ratio of 2,4-dinitrofluorin benzene to zinc power was 1∶4,mol ratio of ethanol to water in the mixed solvent was 3∶2 under refluxing at 50—(60 ℃),the yield reached 70.1%.
2008 Vol. 25 (3): 271-272 [
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3715
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273
Recovering Deteriorated Heat-Conducting Oil by Centrifugal Sedimentation Method
QI Yan-wei~
Deteriorated heat-conducting oil used in TA hydrotreating plant is recovered by centrifugal sedimentation method.Effect of centrifugal time,centrifugal rotational speed on acid number,gum content and solid impurity of the recovered heat-conducting oil were investigated,and the optimum process condition was obtained.Experimental result showed that this method can obviously reduce acid number,solid impurity and gum content of the heat-conducting oil.
2008 Vol. 25 (3): 273-275 [
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276
Preparation of Labetalol
GUO Da-liang,ZHU Xiao-wei
Labetalol was prepared from salicylic amide by five steps: acetylation,bromosubstitution,amino-degradation,condensation and reduction.This approach was stable and easy to control.
2008 Vol. 25 (3): 276-278 [
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1598
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279
Hydrolysis of Lactic-Acid Oligomer in PLA Synthesis
WEI Shun-an,GU Xue-rong
Polylactic acid(PLA) is widely used as a naturally biodegradable material.Ring-opening polymerization of intermediate lactide is the main path to synthesize high molecular weight PLA from lactic acid.In the production of lactide,40% byproduct(oligomer) of the mass was obtained,so how to properly recycle the oligomer is one of the key steps in the industrialization of PLA.In this paper,based on the experiment and the feature of oligomer,the optimal condition of the hydrolysis of oligomer,such as mass ratio,temperature,pressure,was analysed and the pretreatment method to recycle hydrolitic compound was discussed.The hydrolysis process of oligomer was developed,so oligomer can be recycled and this can lower the cost of the production of PLA.
2008 Vol. 25 (3): 279-282 [
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283
2008 Vol. 25 (3): 283-283 [
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