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05 September 2012, Volume 31 Issue 09
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Advances in non-conventional preparation technology of ionic liquids
LI Zhen,CHEN Jing,XIA Chungu
2012, 31(09): 1861-1870.
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1750
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Large-scale application of ionic liquids depends on the continuous advancement of preparation technology. However, the classic procedure for ionic liquids synthesis is excessively time-consuming and unsuitable for mass production, which restricts industrial application of ionic liquids. Aiming at the key process in ionic liquids preparation, the research progress of the non-conventional techniques for preparation of ionic liquids is summarized. The current ionic liquids preparation technologies, such as microwave, ultrasound, microwave-ultrasound, microreactor and Spinning Tube-in-Tube (STT) process intensification are reviewed. Although important progress has been made in non-conventional preparation technique at this stage, intensive research work is still required in order to establish theoretical guidance, and the development of task-functionalized ionic liquids and green preparation technique should be accelerated.
Research progress of estimation methods for critical parameters of pure substances
WANG Xiaoyan,SI Jilin,ZHANG Da,XIANG Shuguang
2012, 31(09): 1871-1877.
Abstract
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2064
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The critical parameters of pure substances are very important in describing fluid phase behavior,predicting their properties,and developing the equation of state.The accuracy of critical parameters directly affects the estimation of other parameters. Through establishing the mathematical model for a limited number of critical parameters is an important research approach to obtaining critical parameters.A variety of estimation methods for critical parameters of pure substances are summarized,including the method of correlating the critical parameters with other properties,group contribution method,method based on liquid equation of state,quantitative structure property relationship (QSPR) method and several types of representative estimation methods of critical parameters are discussed in terms of principles,application ranges,advantages and disadvantages,and development in recent years.The development trend of the methods for estimation of critical parameters is discussed.
Progress of applications of Taylor-vortex flow reactor
YE Li,CAI Xiaoshu,TONG Zhengming
2012, 31(09): 1878-1884.
Abstract
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2126
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As a new type of reactor built on the basis of Taylor-vortex flow theory, Taylor-vortex flow reactor has been used more and more intensively, exhibiting favorable application potential. The influences of operational parameters, such as rotating speed of inner cylinder, axial speed of medium, radius ratio and aspect ratio, on the performances of Taylor-vortex flow reactor are analyzed. Present applications of Taylor-vortex flow reactor in the fields of particle preparation, photocatalysis and cell culture, etc. are introduced. Exisiting application problems, including gas access, flow character improvement and reactor’s scale up, are proposed. Appropriate scale up technologies and studies on reliability of scale-up reactors should become research emphases in the future.
Research and application progress of magnetically stabilized fluidized bed
LIN Tianming,JING Guohua
2012, 31(09): 1885-1890.
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3263
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Magnetically stabilized fluidized bed (MSFB) is a new type of reactor, which combines the advantages of both fixed bed and traditional fluidized bed, and has a great application prospect. In this paper, the progress of basic research and application of MSFB is reviewed. The basic research includes effects of fluid flow rate and magnetic field intensity on fluidization behavior of the magnetic particles in the column, bed voidage, operation stability and transfer characteristics. The application fields include biochemical engineering, energy and environmental engineering. Finally, the existing drawbacks of MSFB are presented. It remains difficult to find the relevant magnetic catalyst in a specific reaction system. MSFB can not be operated at a temperature higher than the Curie temperature of magnetic carrier. The heat generated by the magnetic field generator has an effect on the magnetic carrier and the reaction process and it is difficult to determine the stable operating zone of MSFB. The main research directions of MSFB in the future are proposed, including research and development of magnetic catalyst,stability criterion,mechanism of heat transfer and mass transfer,mechanism of strengthening reaction process,scale-up of reactor and design of industrial reactor.
Research progress of supercritical carbon dioxide dyeing technology
ZHU Yongren,WANG Xunming
2012, 31(09): 1891-1898.
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2308
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The dyeing mechanism of supercritical fluid and different dyeing process conditions are reviewed. Research progress of dyestuffs and color combination of blended dyestuffs is presented. The study on thermodynamics and kinetics of supercritical carbon dioxide dyeing is discussed. Dyestuffs solubility in supercritical carbon dioxide,dyestuffs distribution between fiber and supercritical CO2,and dyestuffs diffusion behavior in fiber are analyzed. The progress of dyeing equipment worldwide is reported. The key problems to be resolved in commercialization of supercritical carbon dioxide dyeing technology are as follows. One is enhancing dyes’ dissolution in supercritical carbon dioxide and diffusion in fiber,the other is development of large volume dyeing kettle under high pressure operating conditions.
Removing copper ion from seawater with redox method
XIE Lixin,TIAN Zhiguo
2012, 31(09): 1899-1902.
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2115
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Anti-corrosion performance of aluminum alloys used in the equipment of seawater desalination can be improved by reducing the concentrations of heavy metal ions in seawater. Removal of Cu2+ in seawater using 5052 aluminum-alloy rings filled in an ion-exchange column as the reducing agent was studied with the redox method. The effect of such factors as temperature,velocity of seawater and initial concentration of Cu2+ in seawater was studied. The surface of aluminum alloys was also characterized by X-ray powder diffraction and scanning electron microscopy. The results showed that 88% of Cu2+ in the seawater can be effectively removed. The efficiency of removing Cu2+ from seawater increased with increasing temperature of seawater and decreasing velocity of seawater. Higher initial concentration of Cu2+ in seawater reduced the efficiency of removal of Cu2+.
Investigation of mini-reformer for hydrogen production
MI Jie1,SUN Guobing1,2,PAN Liwei2,NI Changjun2,ZHANG Lei2,WANG Shudong2
2012, 31(09): 1903-1907.
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2295
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A compact reactor with coupled reactant preheating,methanol steam reforming (MSR),catalytic combustion and water gas shift (WGS) was fabricated to supply hydrogen for PEMFC. The effects of reaction temperature,methanol gas space velocity (GSV) and ratio of water to methanol on reforming reaction were investigated,and the stability of the mini-reformer was also studied under various operation conditions. The yield of hydrogen reached 90L/hr,able to provide hydrogen for 100W PEMFC.
Research on the LNG dense gas diffusion: A continuous horizontal jet release
TANG Jianfeng1,CAI Na1,2,GUO Qing1,WANG Dengdeng1,3
2012, 31(09): 1908-1913.
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2150
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Horizontal jet continuous release was studied through SLAB steady plume dispersion model. The concentration field, temperature field and other characteristics were calculated and analyzed. A MATLAB based program was developed to simulate the continuous leakage diffusion. The characteristics of the diffusion cloud under two different environment conditions were calculated. The environmental conditions included different wind speeds, temperatures, atmospheric stabilities, relative humanities and surface roughness. Changing trends of the diffusion clouds were predicted.
Flow field simulation of supercritical carbon dioxide extractor based on ANSYS Workbench and FLUENT and its structure improvement
GUO Jianzhang1,ZHAO Peng1,WANG Weiqiang2
2012, 31(09): 1914-1918.
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2503
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The shortcomings of the traditional supercritical carbon dioxide extractor are as follows: low space utilization ratio of the extractor owing to the extraction basket occupying the cylinder volume; bad mass transfer and heat transfer owing to the gap between extraction basket and cylinder wall. Aiming at the shortcomings, the extractor structure was improved. Double head structure and radial inlet way were adopted, and a filter screen was set up on the head. Based on ANSYS Workbench and FLUENT, the flow field and temperature field of the improved extractor was simulated at both load and zero load. The simulation results were compared in different situations. The results showed that the improved structure promoted the space utilization ratio and improved the uniformity of flow field and temperature field.
Computation of classifier cut size based on analysis of particle tracks
YUE Daxin,DIAO Xiong,LI Shuangyue,HUANG Peng
2012, 31(09): 1919-1925.
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2454
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In order to study the cut size of a superfine classifier, computational fluid dynamics was used to simulate the gas-solid two-phase flow in the classifier. The RNG k-ε turbulence model was adopted to describe the gas phase, and the particle stochastic trajectory model was used to describe the solid phase. The physical mechanism of particle movement and the classification process in a superfine classifier was revealed by analyzing the relationship between particle tracks and cut size. By analyzing the change of cut size, the effects of rotational speed, air volume, feeding concentration and material density on cut size were established. The results showed that in the theoretical calculation of cut size, ignoring the effect of blade thickness would lead to overly small calculated value. When rotational speed was low (450 r/min,600 r/min), the simulation value and calculated value had a large difference due tor the effect of local turbulence, and the max error was 13.58%. Compared with air volume, the effect of rotational speed on cut size was much more significant. The simulation cut size value agreed well with theoretical calculation. The results provide a new method of obtaining the cut size of a superfine classifier.
Removal and utilization of organic acids in bio-oil
JIANG Hongming1,2,ZHAO Zengli1,CHANG Sheng1,LI Haibin1
2012, 31(09): 1926-1935.
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1790
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Bio-oil,produced by fast pyrolysis of biomass,is an important source of fuel and chemicals. The organic acids in bio-oil are not only the main materials resulting in corrosion in the process of its fuel usage,but also a class of chemicals that can be utilized. The existence form,formation mechanism and the removal and usage of the organic acids in bio-oil are reviewed,and the advantages and disadvantages of different methods,as well as the present status of technologies are analyzed. Overall,it is proposed that development of efficient and stable catalysts for catalytic esterification should be the research focus of removal of organic acids in bio-oil,while direct conversion of organic acids in bio-oil to high value-added chemicals is a preferable way for their utilization.
Formation of thoughts thread and development status quo for exergy transfer study
CHENG Qinglin,LIU Yang,XIANG Xinyao
2012, 31(09): 1936-1941.
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1490
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In accordance with the exergy transition of different types and exergy transfer of identical form,exergy transfer study aims at realizing dynamic adjustment and control for transfer process by investigating its variation and influence factors. Exergy transfer and energy transfer constitute the integrated energy study system. Exergy transfer is closely related with its corresponding nonequilibrium potential field,and is the indispensable dynamics supplement for exergy analysis. Exergy transfer can be extended to describe displacement mechanism of multi-field synergy. Exergy transfer should focus on engineering application and more research on the internal mechanisms of exergy transfer coefficient and parameter system of multi-field synergy for exergy transfer process should be done.
Research on direct conversion of xylose to furfural in high temperature water
SUN Xiaoyin1,DANG Jie2,HUA Derun2,LI Panpan2,WU Yulong2,YANG Mingde2,LI Chun1,3
2012, 31(09): 1942-1945.
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2158
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Direct conversion of xylose into furfural in high-temperature water (HTW) was carried out in a self-made high-pressure reactor. The effect of HTW as the reaction medium on xylose conversion and furfural yield was investigated,and was compared with others catalyst used in the literature. The effects of different solvents on the extraction of furfural were studied. The result showed that HTW was a perfect catalyst medium,which could replace liquid acid and solid acid in the conversion of xylose into furfural. The optimal furfural yield of 78% was obtained at a reaction temperature of 200 ℃,a holding time of 3 h and initial xylose concentration of 10%. In addition,furfural could be well extracted by n-butyl acetate. Therefore,a novel approach to furfural production is presented,providing a basis as well as technical parameters for its commercialization.
On-line resistance measurement for all vanadium redox flow battery by transient-boundary voltage method
PAN Jianxin1,2,LIAO Lingzhi1,XIE Xiaofeng2,WANG Shubo2,WANG Jinhai2,SHANG Yuming2,ZHOU Tao1
2012, 31(09): 1946-1949.
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2229
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A single cell of vanadium redox flow battery (VRB) was investigated on-line by the transient-boundary voltage method. An equivalent circuit model was established using the voltage source,resistor,and a resistor in parallel with the capacitance of three-part series. The effects of current density and state of charge (SOC) on equivalent circuit components values were investigated. The experimental results showed that the polarization resistance decreased slightly with increasing current density,and reached its maximum in the beginning of charge and the end of discharge. Compared with polarization resistance,ohm impedance in the charge/discharge process was the highest respectively 1.905Ω?cm2 and 2.139 Ω?cm2. It was the main factor leading to voltage loss. The transient boundary voltage method is a simple and effective way of characterizing performance of vanadium redox flow battery.
Process for the preparation of copper containing zeolites by solid state ion-exchange method
NING Huiqing1,LU Xinglu2,LIU Quan2,REN Jun2,LI Zhong2
2012, 31(09): 1950-1958.
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2096
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Solid-state ion exchange (SSIE) is a simple and effective method to introduce metal ions into the zeolite framework,which can overcome many adverse factors related to the aqueous ion-exchange method. This work introduces the mechanism of SSIE,the influence of preparation parameters,as well as the application of different types of Cu(Ⅰ) zeolites. The authors propose the preparation of Cu(Ⅰ) zeolites by microwave heating in view of the advantage that the movement of ions is significantly accelerated in the microwave field. The novel preparation method is of great significance in overcoming the difficulty related to the conventional heating method,enhancing ion-exchange degree and removing the influence of residual CuCl,so as to obtain highly efficient Cu(Ⅰ) zeolites.
Progress of catalytic cracking of endothermic fuels
SUN Daoan,LI Chunying,DU Yongmei,ZHANG Wei,Lü Jian
2012, 31(09): 1959-1967.
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2323
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Supersonic flight,the sign of the level of science and technology of a country,is the latest advanced technology in the territory of aerospace. Endothermic fuel is a core technology of supersonic flight. Research history of endothermic fuel is presented. Endothermic fuel and heat sink,catalysts,coking and mechanism of catalytic cracking are reviewed. Zeolite catalyst is one of the most promising catalysts for catalytic cracking of endothermic fuels. However,basic research including selection of endothermic fuels,improvement of zeolite catalysts and catalyst coking,and engineering application research including catalyst loading and simulation of real working conditions are still challenges to application of endothermic fuels. Studies on catalytic cracking mechanism are still weak at present. Microcosmic effect of catalysts and morphology changes are not combined on the molecular scale in the research.
Catalytically stable active phases of transition metal sulfides
LIU Yongjun
2012, 31(09): 1968-1974.
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1727
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The study on catalytic phases and hydrotreating mechanism of transition metal sulfide (TMS) catalysts used in production of clean fuels has received considerable attention. In this paper,the importance of study on catalytically stable active phases of TMS catalysts is emphasized,and the existence and role of carbon in catalytic stable states are summarized and some novel catalytically stable active phases,such as MoSxCy and CoMoC/NiMoC are presented and discussed. At Last,it is pointed out that the conventional CoMoS may be not a catalytically stable active phase but only a precursor,and that some hydrotreating catalysts such as transition metal carbide and TMS may well possess an uniform MoSC-like active phase stucture under catalytical conditions.
Solid superacid catalyst S2O82―/ZrO2-TiO2- Al 2O3 for preparation of levulinic acid
LIU Tao,LI Lijun,LIU Liu,LI Guo,LI Wei,QIN Gui
2012, 31(09): 1975-1979.
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1804
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With sucrose as raw meterial,levulinic acid was preparated by using S2O82―/ZrO2-Ti2O3-Al2O3 as solid superacid catalyst. The effects of technological condition, such as catalyst calcination temperature, catalyst dosage, sucrose concentration, reaction temperature, reaction time on the relative yield of levulinic acid were investigated and orthogonal experiment was used to determine the optimum conditions. The result showed that the highest relative yield of levulinic acid was 72.28% under the optimal conditions of catalyst calcination temperature 550 ℃, sucrose concentration 15 g/L, catalyst dosage 15% of the sucrose amount added to the reaction, reaction temperature 200 ℃, reaction time 60 min.
Synthesis and characterization of ultra-fine ZSM-5 zeolite
JIANG Jianzhun,ZHANG Mingsen,KE Li,YANG Jing,WANG Huanru,HUANG Wenqing
2012, 31(09): 1980-1984.
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2894
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The influence of different types of structure-directing agents (SDA),crystallization temperature and content of alumina source on the crystallization of ultra-fine ZSM-5 zeolite was studied. Scanning electron microscope (SEM),transmitting electronic microscopy (TEM) and X-rays diffraction (XRD) techniques were used to characterize the morphology of the ultra-fine zeolite. The results indicated that the type of SDA had great influence on the crystallization of zeolite. Tetrapropylammonium hydroxide (TPAOH) acted as an excellent SDA for the preparation of ultra-fine ZSM-5 zeolite. Comparatively,the proper temperature for the static crystallization of ultra-fine crystals was in the range from 70 ℃ to 120 ℃ with TPAOH as the SDA. The existence of alumina in the sol-gel inhibited the formation of the crystal nuclei of ZSM-5 zeolite. As a result,without the addition of alumina source,crystallization of zeolite was much faster than that with the existence of alumina source,while an increase in the content of alumina source led to slower crystallization and a much smaller crystal size of zeolite crystallized at the same time of crystallization.
Synthesis of methyl acetoacetate from acetone and dimethyl carbonate over Mg/Al mixed oxides
WANG Dengfeng1,ZHANG Xuelan1,BAI Dong2,LIU Shuyin1,WEI Wei3,SUN Yuhan3
2012, 31(09): 1985-1989.
Abstract
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2338
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A series of Mg/Al mixed oxides with different Mg/Al mole ratios were prepared by calcining hydrotalcite obtained via the co-precipitation method followed hydrothermal treatment. The samples were characterized by using ICP,XRD,CO2-TPD and N2 adsorption/desorption techniques. The results showed that the structure and basicity of samples were affected by Mg/Al mole ratio. Besides,these Mg/Al mixed oxides were effective catalysts for the synthesis of methyl acetoacetate from acetone and dimethyl carbonate. More importantly,they all presented much higher catalytic ability than the pure MgO or Al2O3. At the same time,the catalytic performance of mixed oxides was correlated with their moderate basicity,and the catalyst exhibited the highest catalytic ability when the initial Mg/Al mole ratio was 2. Furthermore,reusability test indicated that these Mg/Al mixed oxides presented good stability and reusability.
Progress of surface grafted nano cellulose whiskers and their liquid crystals
YANG Jie,YE Daiyong
2012, 31(09): 1990-1997.
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2236
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Nano cellulose has received much attention as a new nano biomaterial. Surface grafting modification of nano cellulose is used to develop new functional nanomaterials. The surface grafting methods of nano cellulose whiskers (NCW) are reviewed,such as conventional free radical graft copolymerization,ionic and ring opening graft polymerization and living radical polymerization,which includes nitroxide-mediated polymerization (NMP),atom transfer radical polymerization (ATRP),reversible addition–fragmentation chain transfer polymerization (RAFT) and single electron transfer living radical polymerization (SET-LRP). The application of click chemistry in the surface grafting modification of NCW is summarized. The formation of lyotropic liquid crystal and thermotropic liquid crystal is also discussed. The formation mechanism and the factors affecting cholesteric liquid crystals of NCW are discussed.
Preparation of micro/nano encapsulated phase change materials(PCM)and application to building
YANG Chunxiao,XIE Delong,SITU Yue,HUANG Hong
2012, 31(09): 1998-2005.
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2394
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Micro/nano encapsulated PCM has played an increasingly important role in energy science and other fields. In this paper, preparation of micro/nano encapsulated PCM is reviewed. Preparation methods of micro encapsulated PCM (MEPCM) mainly include interfacial polymerization, in situ polymerization, coacervation suspension polymerization etc. Preparation methods of nano encapsulated PCM (NEPCM) mainly include miniemulsion polymerization and in situ polymerization. Applications of micro/nano encapsulated PCM in modern buildings, such as concrete, wall, wallboard and floor board are described. Present existing problems and the corresponding solutions in the use of micro/nano encapsulated PCM are discussed, such as PCM could not complete full phase change cycles at a high temperature in summer. The future key research directions could be optimizing the synthesis process, strengthening the physicochemical properties of the capsule, and improving its compatibility with inorganic building materials.
Research progress of polypropylene adhesion promoter
QIAO Zemin1,HUANG Zhifeng1,LI Yu2,TANG Hanliang3,LUO Hui3
2012, 31(09): 2006-2010.
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1581
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The recent development of polypropylene adhesion promoter is reviewed,including modification of chlorinated polypropylene,chlorine-free adhesion promoter and waterborne adhesion promoter. The modification of chlorinated polypropylene with unsaturated anhydride and the preparation of chlorine-free adhesion promoter are introduced. Mechanical method,phase inversion technique,spontaneous emulsification method and emulsion polymerization technique are used to prepare waterborne adhesion promoter,and the characteristics of each methods are presented. The application of controlled radical polymerization is also summarized. The compatibility between topcoat and chlorine-free adhesion promoter and the stability of waterborne adhesion promoter should be improved in further study.
Preparation and application of functional acrylate latex
WANG Xiaowen,HE Yufeng,WANG Rongmin,WANG Junfeng,LI Chen
2012, 31(09): 2011-2018.
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1546
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The application of methods and techniques, such as core-shell emulsion polymerization, latex interpenetrating polymer network, soap-free emulsion polymerization, micro-emulsion and mini-emulsion to preparing functional acrylate emulsion is reviewed. The progress of functional acrylate emulsion modified by organic silicon, organic fluoride, polyurethane and epoxy resin, is summarized. Moreover, the application of functional acrylate emulsion, such as functional coatings, adhesive, and leather finishing agents is also introduced. Finally, the development trend of functional acrylate emulsion is proposed. The water-based functional emulsion with high added value, excellent performance and environment-friendliness is the main development direction of the acrylate emulsion.
Research progress of polynitrogen anion N5-
XU Cheng,BI Fuqiang,GE Zhongxue,FAN Xuezhong,WANG Bozhou,WANG Wei,LIU Qing
2012, 31(09): 2019-2023.
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1809
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Polynitrogen anion N5- is an important intermediate in the synthesis of N5+N5-,an energetic material. The synthesis,reaction mechanism,characterization and stability of arylpentazoles were summarized,and the efforts to obtain N5- by dearylation of arylpentazoles were also discussed. It was found that arylpentazoles were synthesized successfully using arylamines as starting material and characterized by means of Raman spectroscopy,NMR and single crystal X-ray diffracion analysis at a low temperature. The effect of substituted groups and solvent on the stability of arylpentazoles were investigated,and the signal of N5- was detected by electrospray ionization mass spectrometry and laser desorption ionization mass spectrometry in negative-ion mode. However,it was concluded experimentally that it was difficult to obtain N5- by chemical methods because of the bad stability of arylpentazoles.
Development of poly (L-lactide) microspheres in high-voltage electrostatic antisolvent process
CHEN Aizheng1,2,YANG Yuemei1,WANG Shibin1,2,SUN Qingqing1,LIU Yuangang1,2,DANG Tingting1
2012, 31(09): 2024-2030.
Abstract
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1935
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An antisolvent,absolute ethyl alcohol was used in the high-voltage electrostatic antisolvent process to prepare poly (L-lactide) microspheres. A 24 factorial experiment was designed to investigate and identify the relative significance of the processing parameters on particle size and particle size distribution of the products. The results indicated that the effect of push speed was dominant in the results regarding particle size. After optimization,the resulting poly (L-lactide) microspheres exhibited good spherical shape,smooth surface and narrow particle size distribution. When the concentration and molecular weight of poly (L-lactide) were 3% (w/v) and 50~100 kDa respectively,the resulting microspheres showed good spherical shape. Fourier transform infrared (FTIR) spectroscopy measurement found no significant structural perturbation. X-ray powder diffraction (XRPD) analysis revealed no significant crystal structural changes.
Removing organic pollutant with microbial red mud porous material
WANG Xiaoyu1,WANG Xiaolong2,WU Limei1,Lü Guocheng1,HE Wenhui1
2012, 31(09): 2031-2035.
Abstract
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1973
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In this study,a porous material was prepared from red mud (bauxite residue) and other industrial waste. The porous material was modified by acid,alkali or zirconium oxychloride and was loaded with pseudomonas putida to remove phenol in sewage. The strength of porous material nodulized at 1200 ℃ could meet the test requirements. Its porosity reached 80%,and pore size was controlled between 50 and 100 nm. Porous material modified by zirconium oxychloride had higher loading capacity for pseudomonas putida,than the porous material modified by acid or alkali and unmodified original red mud. The main factors that affected phenol removal were solution pH and initial phenol concentration. The optimum condition was solution pH at 5~6 and initial concentration of phenol at 40 mg/L. Removal rate could reach 80% under the optimum condition.
Ultraviolet mutagenesis breeding and fermentation conditions of phospholipase D producing strain
LIU Yuanyuan,ZHANG Xiaoli,YAO Na,Li Hongya,Zhao Binxia
2012, 31(09): 2036-2038.
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1679
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Phospholipase D (PLD) catalyzed transphosphatidylation reaction plays an important and useful role in synthesis of phospholipids. In the present paper,a PLD-high-producing strain was selected by ultraviolet mutagenesis from wild Streptomyces and its PLD activity was increased by 42.5% against the original strain. The PLD producing conditions for the mutant strain was investigated in shake flask fermentation. The optimized components (g/L) of culture medium were 10.0 of glucose,5.0 of beef extract,5.0 of peptone,1.0 of MgSO4?7H2O,3.0 of CaCl2,and 2.0 of NaCl. The enzyme productivity could also be enhanced by the supply of surfactant i.e. Tween 80,and its optimal concentration was 0.6 g/L. Under the above conditions,3.23 U/mL of enzyme activity was achieved in 500 mL of shake flask fermentation.
Research progress of chemical synthesis of myrcene
YANG Yang1,YOU Yahua1,YAO Risheng2,3
2012, 31(09): 2039-2042.
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1865
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Myrcene is a widely used fragrance and flavor raw material and intermediate. The progress of chemical synthesis of myrcene, such as from the esters of isopentanoids, monoterpenes allyl acetate and isoprene is reviewed. Especially, myrcene is synthesized by dimerization of isoprene due to its low cost, easy access and effective utilizationse of C5 resource. Finally, the future development for chemical synthesis of myrcene is proposed. The main research directions are to develop new catalysts, optimize technology and route of the reaction, and improve the yield and selectivity of myrcene.
Progress of synthesis and application of hydroxylamine (salts)
GAO Liya,TAN Xuejun,ZHANG Dongsheng,WANG Shufang,ZHAO Xinqiang,WANG Yanji
2012, 31(09): 2043-2048.
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2422
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The industrial routes,such as Raschig synthesis,reduction of nitrous acid,and one-pot synthesis for preparation of hydroxylamine (salts) are reviewed. Furthermore,the new application of hydroxylamine to synthesis of aniline and phenol derivatives,along with traditional uses of hydroxylamine (salts) for the production of cyclohexanone oxime and hydroxylamine-O-sulfonic acid,is also introduced. With increasing demand for hydroxylamine,future trend on hydroxylamine (salts) synthesis is proposed based on the above discussions,i.e. one-pot synthesis of hydroxylamine can be realized efficiently under mild reaction conditions.
Synthesis of MOPBG-AMPS copolymer and evaluation of inhibition of barium sulfate scale
WEI Xiaofei,WANG Minggang
2012, 31(09): 2049-2052.
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1910
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A water-soluble MOPBG-AMPS scale inhibition agent was prepared from N,N-(2-methylene-1-oxo-1,3-propanediyl)-bis-glycine (MOPBG) and 2-acrylamido-2-methyl propane sulfonic acid (AMPS) in aqueous solution using persulfate as initiator. The structure and thermal stability of the copolymer was characterized by FTIR and TGA. Using the static experiment method,the inhibition of BaSO4 scale was studied. The results showed that the copolymer [n(MOPBG)∶n(AMPS)=3∶(1.5—2)] showed the best heat resistance. As an excellent scale inhibitor,the inhibition capability of copolymer [n(MOPBG)∶n(AMPS)=3∶1.5] reached 98.9% at the dose of 20 mg/L,the inhibition capability of copolymer [n(MOPBG)∶n(AMPS)=3∶2] reached 96.4% at the dose of 15 mg/L. Formation of BaSO4 crystals was determined by SEM,and the mechanism of scale inhibition was discussed.
Synthesis and application of α-methyl styrene dimer
SONG Guoqiang1,JIN Xiaobei1,HU Chunqing2, CHEN Xin1
2012, 31(09): 2053-2057.
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2099
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Linear dimer, product (Ⅰ) and cyclic dimer, product (Ⅱ) of α-methyl styrene(α-MS) were synthesized with high selectivity from α-MS, and macromolecular photoinitiator KIP150, product (Ⅲ) was prepared from α-MS cyclic dimer in two steps. The results indicated that in the presence of p-toluenesulfonic acid, the yield of product (Ⅰ) was more than 88.0% and the purity was up to 99.8% at reaction temperature 30 ℃ for 24h. Moreover, in the presence of p-toluenesulfonic acid and at reaction temperature 100 ℃ for 7h, the yield of product (Ⅱ) was up to 98.0% and the purity was more than 99.8%. The yield of product (Ⅲ) was more than 70.0% when synthesized via Friedel-Crafts acylation and hydroxylation reaction with α-MS cyclic dimer, and the purity was up to 95.0%. The products and intermediates were characterized by LC-MS, 1H NMR, GC and HPLC.
Preparation of high temperature resistant anaerobic adhesive and its storage life
PENG Xiaoqin1,CHEN Liang2,CHEN Bingyao3,LING Hui2,LI Jun2
2012, 31(09): 2058-2063.
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1891
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With ethoxylated bisphenol A dimethacrylate (BPA2EODPT) and epoxy acrylate (EA) and trimethylolpropane trimethacrylate (TMPTMA) as raw materials,N,N'-4,4'- diphenylmethyenebismaleimide (BMI) and gas phase silicon dioxide(SiO2) as heat resistant modifier,cumene hydroperoxide (CHP) as initiator,N,N-diethyl-p-toluidine and saccharin as main accelerant and secondary accelerant respectively, p-benzoquinone (BQ) and tetrasodium EDTA (Na4EDTA) and hydroquinone (HQ) as stabilizer,the formula of anaerobic adhesive was optimized. The properties of the anaerobic adhesive were better because of its good heat resistance and storage stability when mass ratio of m(BPA2EODPT)︰m(EA)︰m(TMPTMA) was 3.1︰1︰2.5,mass fractions of BMI and SiO2 were 6% and 4% respectively,mass fractions of DPT and SA were 0.4% and 2% respectively,mass fractions of BQ and Na4EDTA and HQ were 0.07% and 0.04% and 0.11% respectively.
Properties of aqueous solutions of cationic polyacrylamide with quaternary ammonium group
TENG Xiaoxu1,SHI Jianwei,ZHANG Shufen2
2012, 31(09): 2064-2069.
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2175
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As a cationic agent,cationic polyacrylamide with quaternary ammonium group is used for pretreatment of cotton fabrics and the pretreatment results were influenced by the solution properties of the cationic agent. The viscosity and conductivity of the cationic agent were investigated,and the results were proven by the salt-free dyeing data of the cationic cotton. It was indicated that the value of reduced viscosity of the cationic agent with a low molecular weight was smaller,and the molecules of the cationic agent could be well distributed on the pretreated cotton,and good levelness of the dyed cotton was obtained. The number of the positive charges on the cotton pretreated with the cationic agent with high cationic degree increased because of its stronger ionizing power in aqueous solution,and the K/S value of the dyed cotton also increased.
Preparation of 4,4'-diaminostilbene-2,2'-disulfonic acid by Pt/C catalytic hydrogenation
ZHANG Junhua1,GUO Haiguang1,HUAN Changyong1,JIANG Li2,SHEN Qiang1
2012, 31(09): 2070-2074.
Abstract
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1667
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Preparation of 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) with the liquid-phase catalytic hydrogenation method using Pt/C as catalyst in water medium was studied. The optimum technical conditions determined by a series of experiments were as follows: 60 g (wet) of feed material DNS,200 mL of H2O,0.3 g (dry) of catalyst 3%Pt/C,reaction temperature of 45—50 ℃,reaction pressure of 0.5—0.65 MPa and pH value of 5—7 in the reaction system. Under these optimum technical conditions,purity of the product could exceed 99%,by-products of benzyl and aldehyde compounds were less than 0.15%. The yield of product came up to 98.5%. And,through a proprietary catalyst regeneration technology,the catalyst could be reused more than 20 times,reducing the cost greatly and providing the foundation for its commercialization.
Current status and outlook of carbon dioxide mineral carbonation technologies
ZHANG Bingbing1,WANG Huiming1,ZENG Shanghong2,SU Haiquan1,2
2012, 31(09): 2075-2083.
Abstract
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1957
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Facing the ecological disaster caused by greenhouse effect, the key is to seal the huge carbon dioxide using various CO2 storage technologies. Carbon dioxide mineral sequestration is one of the most environment-friendly, secure and permanent technology. This paper introduces the basic principle of CO2 mineral carbonation in terms of sequestration solutions, reaction kinetics and carbonation materials, and various process routes of CO2 mineral carbonation are described, including direct mineral carbonation and indirect mineral carbonation, such as acid extraction, molten salt process, ammonia extraction and bioleaching. Meanwhile, combined with the research and development of CO2 mineral carbonation techniques both in China and the rest of the world, the advantages and disadvantages of present researches and commercialization prospect are also discussed. Moreover, it is proposed that the next key point of research and development of CO2 mineral carbonation techniques is to pay more attention to resources utilization, regarding CO2 as cheap carbon source, and promoting carbon capture, utilization and sequestration (CCUS) project.
Technology status and analysis on coal-fired flue gas denitrification
GU Weirong,ZHOU Mingji,MA Wei
2012, 31(09): 2084-2092.
Abstract
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2482
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The technology status and analysis on coal-fired flue gas denitrification were reviewed. The selective catalytic reduction (SCR),selective non-catalytic reduction (SNCR),SNCR-SCR and their industrialization status were analyzed,the new technologies for control NOx both at home and abroad were introduced,finally the development of the denitrification technology should be to develop the techniques with Chinese characteristics and enhance the development of new denitrification technologies .
Sodium peroxydisulfate activated by zero-valent iron for degradation of methyl orange
YANG Meimei1,ZHOU Shaoqi1,2,3,ZHENG Yongxin1,ZHENG Ke1
2012, 31(09): 2093-2096.
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2553
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Oxidative degradation of methyl orange (MO) in aqueous solution by zero-valent iron-activated sodium peroxydisulfate (PDS) was investigated. The degradation process was based on generation of sulfate radicalsas powerful oxidizing species. The effects of dosages of PDS and Fe0,initial pH,temperature and initial concentration of MO on MO degradation were examined in batch experiments. The results demonstrated that MO could be degraded by Fe0/PDS reagent effectively. Under the condition with initial MO concentration 100 mg?L-1,PDS dosage 0.912 mmol?L-1,Fe0 dosage 0.16 g?L-1,pH 4.0,temperature 298 K,MO degradation in aqueous solution reached 80.2% within 2.5 h. At the same time,the kinetics of Fe0/PDS system oxidation of MO was investigated, and the results demonstrated that degradation of MO occurred in two stages, and the second stage of the reaction followed first-order kinetics behavior.
Ultrasound-enhanced adsorptive removal of PFOS and PFOA by granular activated carbon
ZHAO Deming1,ZHANG Dexing1,HOFFMANN Michael R2
2012, 31(09): 2097-2101.
Abstract
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7967
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The adsorption of perfluorooctane sulfonate (PFOS) and perfluorooctanoate (PFOA) from Milli-Q water(MQ) and landfill groundwater (GW) by granular activated carbon (GAC) in the absence and presence of 20 kHz ultrasound was investigated. The equilibrium adsorption isotherms were well described by the BET multilayer absorption isotherm and maximum monolayer sorption capacity was qmPFOS>qmPFOA. In all cases,the adsorption kinetics were well represented by a pseudo-second-order model,with equilibrium sorption capacity and initial sorption rate values following the order qePFOS>qePFOA and hPFOS>hPFOA,respectively. The equilibrium PFOS and PFOA adsorption constants,qe and qm,and the adsorption kinetic constants,h and K,were greater in Milli-Q water(MQ) than landfill groundwater (GW) with or without pretreatment,indicating competition for adsorption sites by groundwater organics. Ultrasonic irradiation significantly increased the PFOS/PFOA-GAC adsorption kinetics,by an enhanced factor of 7.7 and 4.4 respectively.
Catalytic distillation coupled with a side reactor for methyl acetate hydrolysis
ZHENG Huidong,ZHAO Suying,ZENG Yanru,WANG Liang’en,XU Binghui
2012, 31(09): 2102-2106.
Abstract
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2395
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An experimental setup of catalytic distillation coupled with a side reactor was established to hydrolyze methyl acetate with high conversion rate. The influences of operating parameters on the conversion rate and the mass ratio of acetic acid to water were investigated. This new technology was also compared with traditional single column catalytic distillation. The results showed that the molar ratio of water to methyl acetate had a great impact on the conversion rate of methyl acetate. With the increase of the volume ratio of reflux to methyl acetate feed the conversion rate of methyl acetate slowly increased and energy consumption linearly increased,and the optimum volume ratio of reflux to methyl acetate feed was 3.0. Due to a slow decrease of conversion rate of methyl acetate with the increase of space velocity,a higher space velocity would be favorable in increasing processing capacity. A bigger fixed reactor can improve the conversion rate of methyl acetate at the outlet of the reactor but is not necessarily conducive to higher total conversion rate. This new technology can realize the hydrolysis of methyl acetate with high conversion rate and is better than traditional single column catalytic distillation.
Environment-friendly preparation of tert-butylamine
YAN Jixiao,JIN Yifeng,LIU Zhixiang,WANG Yuefen
2012, 31(09): 2107-2109.
Abstract
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2088
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The environment-friendly preparation process of tert-butylamine by reacting isobutene with ammonia over HZP-II catalyst was studied. The affecting factors on amination were investigated,such as space velocity,reaction temperature,ratio of ammonia to isobutene. In addition,the life of HZP-II catalyst was assessed. Under optimal conditions: reaction pressure 5MPa,reaction temperature 260 ℃,isobutene space velocity 450 h-1,mole ratio of ammonia to isobutene (1.5—3.0)∶1,reaction time more than 2000h,conversion of isobutene and selectivity of tert-butylamine could be up to 10.2% and 99% respectively.
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