Synthesis and characterization of pure mesoporous zirconia thin film with two-dimensional hexago
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酚醛树脂重均分子量酚醛树脂重均分子量引言酚醛树脂作为一种重要的合成材料,在工业和科学领域具有广泛的应用。
它的性能取决于许多因素,其中之一就是重均分子量。
重均分子量是用来描述分子链长度的指标,它会对酚醛树脂的物理和化学性质产生显著影响。
在本文中,我们将对酚醛树脂重均分子量进行深入探讨,旨在帮助读者更好地理解这一概念。
一、酚醛树脂的重均分子量定义及影响因素1.1 定义酚醛树脂的重均分子量是指分子链长度在一定范围内的平均值。
分子链的长度会影响树脂的流动性、机械性能和耐热性,因此重均分子量是酚醛树脂性能的重要指标之一。
1.2 影响因素酚醛树脂的重均分子量受到许多因素的影响,包括酚和醛的摩尔比例、反应时间、反应温度和催化剂的种类等。
这些因素会影响分子链的生长速率和长度分布,最终导致酚醛树脂的重均分子量的变化。
二、酚醛树脂重均分子量的作用及性能影响2.1 作用酚醛树脂的重均分子量对其性能有着重要作用。
较高的重均分子量会使树脂分子链更长、更紧密排列,从而提高了树脂的力学强度和耐热性。
高重均分子量的酚醛树脂还具有较好的电绝缘性能和抗化学腐蚀性能。
2.2 性能影响酚醛树脂的重均分子量直接影响其物理和化学性质。
较低的重均分子量会导致树脂的流动性增加,降低了树脂的机械强度和耐热性。
而较高的重均分子量则可以提高树脂的抗拉强度和耐热性。
三、酚醛树脂重均分子量的测定方法3.1 胶体滴定法胶体滴定法是一种常用的测定酚醛树脂重均分子量的方法。
它基于胶体滴定原理,通过滴定试剂与酚醛树脂中的活性基团反应,从而确定重均分子量的大小。
3.2 溶液粘度法溶液粘度法是另一种常用的测定酚醛树脂重均分子量的方法。
它通过测定树脂溶液的粘度来推算出其重均分子量的大小。
四、个人观点和理解酚醛树脂重均分子量作为描述分子链长度的指标,对树脂的性能有着显著影响。
在制备酚醛树脂时,合理控制重均分子量对于获得具有理想性能的树脂产品至关重要。
在实际应用中,通过调节反应条件和添加助剂可以改变酚醛树脂的重均分子量,从而满足不同领域的需求。
第 41 卷 第 6 期2012 年 6 月Vol.41 No.6Jun.2012化工技术与开发Technology & Development of Chemical Industry用钛白副产硫酸亚铁制备纯磷酸铁及其表征阮 恒1,易均辉2,龚福忠2(1.广西化工研究院,广西 南宁 530001;2.广西大学化学化工学院,广西 南宁 530004)摘 要:以钛白粉生产过程中的副产物绿矾(硫酸亚铁)为原料,通过净化除杂,用双氧水为氧化剂,再加入磷酸、表面活性剂,制备了超细磷酸铁。
用X射线衍射分析(XRD)、差热-热重分析(TGA-DTA)、X射线光电子能谱分析(XPS)、扫描电镜(SEM)和粒度分布测量等研究了样品的物相结构、表面形貌和粒径分布。
结果表明,采用该反应条件有利于控制产物的形貌和粒径,且其产品纯度高。
关键词:绿矾;磷酸铁;物相结构;表面形貌;表面活性剂中图分类号:TQ 126.3 文献标识码:A 文章编号:1671-9905(2012)06-0010-03磷酸铁可作为无毒防锈颜料、催化剂和陶瓷釉面涂料[1~3]。
近年来,在电池领域,磷酸铁作为电池材料如磷酸铁锂材料的原料被广泛研究和应用[4~6]。
磷酸铁可由铁盐和磷酸盐在高温下反应生成,也可由亚铁盐和磷酸盐在氧化剂作用下反应而得。
常用的亚铁盐是硫酸亚铁。
目前我国的钛白粉生产中,每生产1t钛白粉就产生约3.5~4t副产物绿矾(七水硫酸亚铁,分子式FeSO4・7H2O),这些副产物一部分用于饲料添加剂、净水剂、农肥,一部分用于生产氧化铁颜料(如铁红、铁黄、铁蓝、铁黑 )等,但仍有很大一部分无法得到有效利用。
本文以钛白生产副产物硫酸亚铁为原料,先进行净化除杂,然后加入磷酸和双氧水进行反应,得到了超细纯磷酸铁粉体,再以自制磷酸铁为原料,制备了锂电池正电极材料磷酸铁锂,用X射线衍射(XRD)、差热-热重分析(TGA-DTA)、XPS扫描电镜(SEM)和粒度分布测量仪研究了磷酸铁样品的物相结构、颗粒形貌及其粒径分布,为钛白生产副产物硫酸亚铁的利用开辟了新的途径。
3 化工英语文献3.1化工英语文献的结构Title, (Author names, Affiliation),Abstract ,(Keywords),Introduction,Experimental,Results, Discussions (Results and discussions),Conclusions,Acknowledgements,References3.2 英语文献的检索Elsevier—science directSpringerlinkWiley interscience3.3 中英文摘要1、定义以提供文献内容梗概为目的,不加评论和补充解释,简明、准切地记叙文献重要内容的短文。
好的摘要对于增加论文的被检索和引用的机会、吸引读者、扩大影响起着不可忽视的作用。
2、摘要的类型和基本内容类型:根据内容的不同,摘要分为三大类:报道性摘要、指示性摘要和报道-指示性摘要。
1)报道性摘要(informative abstract)。
也称信息性摘要或资料性摘要。
其特点是全面、简要地概括论文的目的、方法、主要数据和结论。
通常,这种摘要可部分地取代阅读全文。
2)指示性摘要(indicative abstract)。
也称说明性摘要、描述性摘要(descriptive abstract)或论点摘要(topic abstract)。
一般只用二、三句话概括论文的主题,而不涉及论据和结论,多用于综述、会议报道等。
帮助读者决定是否需要阅读全文。
3)报道-指示性摘要(informative- indicative abstract)。
以报道性摘要的形式表述一次文献中信息总价值较高的部分,以指示性摘要的形式表述其余部分。
传统的摘要多为一般式,在内容上大致包括引言(introduction)、材料和方法(materials and methods)、结果(results)和讨论(discussion)。
即IMRAD3、EI对摘要的要求《EI》中国信息部要求信息性文摘(Information Abstract)应该用简洁、明确的语言(约300汉字,150 英文字)将论文的“目的(Purposes)”,主要的研究“过程(Procedures)”及所采用的“方法(Methods)”,由此得到的主要“结果(Results)”和得出的重要“结论(Conclusions)”表达清楚。
第35卷第3期2006年3月应 用 化 工App lied Che m ical I ndustryVol .35No .3M ar .2006收稿日期:2005212221作者简介:管 洁(1981-),男,江苏高邮人,浙江大学硕士研究生,师从包永忠教授,主要从事丙烯酸酯聚合物的合成和表征的研究。
电话:(0571)87951334,E 2mail:yongzhongbao@zju .edu .cn甲基丙烯酸甲酯2丙烯酸乙酯乳液共聚动力学研究管 洁,包永忠,黄志明,翁志学(浙江大学聚合反应工程国家重点实验室,浙江杭州 310027)摘 要:为了合成适于药物包衣用的甲基丙烯酸甲酯2丙烯酸乙酯(MMA 2E A )共聚物胶乳,对以非离子型乳化剂OP 210为乳化剂、过硫酸钾为引发剂的MMA 2E A 乳液共聚动力学进行了研究。
发现初期共聚速率随着乳化剂浓度、引发剂浓度和聚合温度的增加而增大,这是由于共聚物乳胶粒子平均粒径随着乳化剂、引发剂浓度和聚合温度的增加而减小,乳胶粒子数目增加所致。
通过调节乳化剂、引发剂以及反应温度可以达到合适的聚合反应速率,最终合成出转化率大于95%的MMA 2E A 共聚乳液。
关键词:甲基丙烯酸甲酯;丙烯酸乙酯;乳液聚合;动力学中图分类号:O 632.52;O 631.5 文献标识码:A 文章编号:1671-3206(2006)03-0192-03Study of ki n eti c of e mulsi on copoly meri zati on of methyl methacryl ate /ethyl acryl ateG UAN J ie,BAO Yong 2zhong,HUAN G Zh i 2m ing,W EN G Zh i 2xue(State Key Laborat ory of Poly mer Reacti on Engineering,Zhejiang University,Hangzhou 310027,China )Abstract:I n order t o synthesize methyl methacrylate 2ethyl acrylate (MMA 2EA )copoly mer latexes suit 2able for the app licati on of drug coating,the kinetics of MMA 2E A e mulsi on copoly merizati on,using OP 210as the e mulsifier and KPS as the initiat or,were investigated .It was found that the initial copoly merizati on rate increased as the concentrati on of the e mulsifier,initiat or and poly merizati on te mperature increasing .It was caused by the increase of latex particles number as evidenced by the decrease of size of latex particles as the concentrati on of the e mulsifier,initiat or and poly merizati on te mperature increasing .MMA 2EA copol 2y mer e mulsi on with high poly merizati on conversi on (>95%)was p repared by adjusting the poly merizati on conditi ons .Key words:methyl methacrylate;ethyl acrylate;e mulsi on poly merizati on;kinetics 药用丙烯酸树脂是由丙烯酸和甲基丙烯酸及其酯以一定比例共聚而成的一类高分子材料,具有安全、稳定、惰性及无刺激等优点,可用作片剂、胶囊和微丸制剂的薄膜包衣材料[1,2]。
JOURNAL OF RARE EARTHS,Vol.27,No.6,Dec.2009,p.895Fou ndation it em:Project s upported by the National Natural Science Foundation of China (20671042,50872045)and the Natural Science Foundations of Guang-dong Province (0520055,7005918)Cor respondin g aut hor:LI Wenyu (E-mail:liwenyu_jnn@;Tel.:+86-20-85221813)DOI 6S ()635Synthesis and char acter ization of Y 2O 2S:Eu 3+,Mg 2+,Ti 4+nanorods via a solvothermal routineLI Wenyu (李文宇),LIU Yingliang (刘应亮),AI Pengfei (艾鹏飞),CHEN Xiaobo (陈小博)(Department of Chemistry,Jinan University,Guangzhou 510632,Chi na)Received 24December 2008;revised 27April 2009Abstract:Y 2O 2S:Eu 3+,Mg 2+,Ti 4+nanorods were prepared by a solvothermal procedure.Rod-like Y(OH)3was firstly synthesized by hydro-thermal method to serve as the precursor.Y 2O 2S:Eu 3+,Mg 2+,Ti 4+powders were obtained by calcinating the precursor at CS 2atmosphere.The Y 2O 2S:Eu 3+,Mg 2+,Ti 4+phosphor with diameters of 30–50nm and lengths up to 200–400nm inherited the rod-like shape from the pre-cursor after calcined at CS 2atmosphere.The Y 2O 2S:Eu 3+,Mg 2+,Ti 4+nanorods showed hexagonal pure phase,good dispersion and exhibited bright red luminescence.After irradiation by 265or 325nm for 5min,the phosphor emitted red long-lasting phosphorescence,and the phos-phorescence could be seen with the naked eyes in the dark clearly for more than 1h after the irradiation source was removed.It was consid-ered that the long-lasting phosphorescence was due to the persistent energy transfer from the traps to the Ti 4+and Mg 2+ions to generate the red-emitting long-lasting phosphorescence.Keywords:yttrium oxysulfide;rod-like structure;nanomaterials;luminescence;rare earthsDuring the recent half-century there have been consider-able interests in the long-lasting phosphors because of their potential applications in safety indicators,fluorescent lamps,urgent illumination system,and cathode ray tubes,etc.[1–4]From the point of practical application,red is one of the three fundamental colors,and a red or orange afterglow phosphor is most suitable as illuminating light sources and appropriate for various displays.Therefore,red long-lasting phosphors with high luminescence and good chemical sta-bility are badly needed.Yttrium oxysulfide has been known for a long time as an excellent red phosphor host material.While doped with Eu,Mg,Ti,a red long-lasting phosphor with the afterglow time of above 3h has been synthesized [5].But until now,the progress on the systemic research of Y 2O 2S:Eu 3+,Mg 2+,Ti 4+is very slow and the luminescent mechanism is not well disclosed.The research of the long-lasting phosphors is mainly fo-cused on the bulk materials.However,one-dimensional rare-earth nanocrystals have recently attracted great attention because of their wide applications in fabrication of optical,electronic,biochemical and medical devices [6–9].If the rare earth compounds were fabricated in the form of one-dimen-sional nanostructures,they would have some new properties as a result of both their marked shape-specific and quan-tum-confinement effects.For luminescent materials,the phosphorescent properties are greatly affected by grain size,and many new properties can be obtained when the grain size reaches nanoscale.There are some methods for the prepara-tion of fine powders in nanosize,including sol-gel method,chemical precipitation,hydrothermal synthesis,and so on.The solvothermal method which exhibits some advantages of low processing temperature,high homogeneity and purity of the products has become a promising method for the prepara-tion of well-crystallized nanomaterials.Recently,some rare earth hydroxides with controlled morphology have been re-ported [10–13].As for lanthanide oxysulfides,only La 2O 2S,Gd 2O 2S and Eu 2O 2S are known as nanorods [14–16],La 2O 2Sand Nd 2O 2S as nanowires [17]and Y 2O 2S as nanotubes [11].There is still great difficulty in developing an effective route to synthesis high-quality (single-crystalline,well-shaped and phase-pure)nanocrystals.Until now the way to produce Y 2O 2S:Eu 3+,Mg 2+,Ti 4+nanorods hasrarely been reported yet.In this paper,we reported that,for the first time to our knowledge,Y 2O 2S:Eu 3+,Mg 2+,Ti 4+nanorods have been prepared by solvothermal method followed by a calcination process in CS 2atmosphere,and their photoluminescent properties were characterized at room temperature.Such Y 2O 2S:Eu 3+,Mg 2+,Ti 4+nanorods showed persistent red:10.101/1002-07210808-0896J OURNAL OF RARE EARTHS,Vol.27,No.6,Dec.2009emission after UV illumination,exhibiting potential in photoluminescent application.1Experimental Firstly,0.091mol Y 2O 3was dissolved in concentrated HNO 3.Then appropriate amount of ammonium aqueous so-lution was added dropwise.The co-precipitated powders were centrifugally separated,washed with distilled water and butanol three times,and then mixed with 40ml butonal.The solution was transferred to a teflon-lined stainless auto-clave and maintained at 260C for 5h and then cooled down to room temperature.The desired white hydroxide nanorods were filtered,washed with distilled water and ace-tone three times,and finally dried at 80C for 6h.In the second place,sulfur powder was put in a sealed graphite cru-cible,and heated to 800C for 4h.Then the dried precursor together with the mixture of 0.005mol Eu 2O 3,0.001mol Mg(OH)2.4MgCO 3.6H 2O,and 0.001mol TiO 2were placed into the graphite crucible and calcined at 1100C for 4h.Both the as-prepared Y(OH)3precursor and the final Y 2O 2S:Eu 3+,Mg 2+,Ti 4+phosphorescent products were characterized.The structures of the products were determined by powder X-ray diffraction (Bruker D8Focus).The morphologies of the powders were observed by employing scanning electron mi-croscopy (SEM,Philips XL-30),transmission electron mi-croscopy (TEM,Philips TECNAI 10)and high resolution transmission electron microscopy (HRTEM,Fei TECNAI G2F20).The photoluminescence spectra and intensity weremeasured on a fluorophotometer (Hitachi F-4500).All meas-urements were carried out at room temperature.2Results and discussion2.1Crystal structure of the product sFig.1shows pure phases of Y(OH)3precursor generated by a solvothermal process and Y 2O 2S after calcined in CS 2environment.It can be seen from the XRD patterns that both Y(OH)3and Y 2O 2S possess hexagonal structures.No impu-rity peaks are observed.As for Y 2O 2S,lattice parameters are as a=0.375nm,c=0.656nm by calculation,which are very close to the standard lattice parameters provided by the powder diffraction file,PDF #24-1424.Co-doped Eu 3+,Mg 2+and Ti 4+occupy the lattice sites in Y 2O 2S structure to form a uniform solid solution,with a nominal chemical composition of Y 2O 2S:Eu 3+,Mg 2+,Ti 4+.2.2Morphology of the Y(OH)3pr ecursorAs shown in Fig.2,Y(OH)3nanorods with uniform size and good distribution are obtained by the solvothermal method,showing the advantage of this method in preparing the particles with uniform size.A TEM micrograph is pre-sented in Fig.2(c),indicating obviously that the surface of the nanorods is smooth.2.3Morphology of the Y 2O 2S:Eu 3+,Mg 2+,Ti 4+nanorods The calcination of the Y(OH)3in CS 2atmosphere leads toFig.1XRD patterns of the obtained Y(OH)3and Y 2O 2S:Eu 3+,Mg 2+,Ti 4+nanorodsFig.2Morphology of Y(OH)3precursor ()S M ;()()T M a E image b and c E micrographsLI Wenyu et al.,Synthesis and characterization of Y2O2S:Eu3+,Mg2+,Ti4+nanorods via a solvothermal routine897the formation of Y2O2S.As shown in Fig.3,all the crystals are of rod-like shape with the width diameters of30–50nm and the lengths ranging from200to400nm.For oxysulfide products,their1D linear morphology and diameters are nearly identical to those of the initial Y(OH)3nanorods,im-plying that the rod-like shape is kept after the high tempera-ture calcination.Although the exact mechanism is not clear now,it should be mentioned that the atmosphere in which the precursor is calcined plays an important part in keeping the rod-like shape.In our previous experiments[18],when the mixture was calcined in a flowing N2,air or H2S environ-ment,only Y2O2S:Eu3+,Mg2+,Ti4+particles were obtained. In this solid-gas reaction under such high temperature,we believe that the atmosphere is a key factor of a close mor-phological retention between the starting Y(OH)3and the final products.The detailed research of the mechanism is under way.2.4HRTEM examination of the Y2O2S:Eu3+,Mg2+,Ti4+nanorodsThe Y2O2S:Eu3+,Mg2+,Ti4+nanorods were also examined by using high resolution transmission electron microscopy. From Fig.4(a)we can see individual nanorods with the di-ameter of about50nm.A HRTEM micrograph of the nano-rod is shown in Fig.4(b),from which the single crystalline nature of the nanorod is confirmed.The spacing between the two adjacent lattice planes is0.365nm,which is just in good agreement with the interplanar crystal spacing of(101)of hexagonal phase Y2O2S:Eu3+,Mg2+,Ti4+.As is revealed in Fig.4(c),the corresponding selected area electron diffrac-tion pattern obtained is quite consistent with the target Y2O2S phase.These results further confirm that the final products are pure phased and single crystalline nanorods.2.5Luminescence property of the synthesized red phosphor For the sample calcined in CS2atmosphere under1100C, the excitation spectrum,shown in Fig.5(a),consists mainly of a wide band with two peaks at about260and325nm corresponding to Eu–O CTB(charge transfer band)and Eu–S CTB.While some weak and narrow peaks are attrib-uted to the f-f transition of Eu3+ions.The emission spectrum (Fig.5(b))excited by325nm indicates typical emission of Eu3+ion.The strong red-emission lines at615and625nm are due to transition from5D0to7F2level of Eu3+ion.Either Ti4+or Mg2+ion does not change the shape of excitation and emission spectra dramatically.2.6Afterglow decay curves of the phosphor sFrom the decay curve in Fig.6,it can be seen that doping both Mg2+and Ti4+ions can result in a long afterglow oftheFig.3Morphology of Y2O2S:Eu3+,Mg2+,Ti4+(a)SEM image;(b)and(c)TEMmicrographsFig.4TEM observation of Y2O2S:Eu3+,Mg2+,Ti4+nanorod(a)TEM micrograph for a single nanorod;(b)HRTEM image of the nanorod,showing single crystalline nature;()S Dc Corresponding AE pattern898J OURNAL OF RARE EARTHS,Vol.27,No.6,Dec.2009Fig.5Excitation and emission spectra of the Y2O2S:Eu3+,Mg2+,Ti4+phosphor(a)Excitation spectrum monitored at625nm;(b)Emission spectrum excited by325nmFig.6Afterglow decay curves of the phosphors(1)Y2O2S:Eu3+nanorods;(2)Y2O2S:Eu3+,Mg2+,Ti4+nanorods Y2O2S:Eu3+phosphor.The single Eu3+doped Y2O2S:Eu3+ phosphor shows very weak afterglow while red afterglow color can be clearly seen in the dark room for codoped Y2O2S:Eu3+,Mg2+,Ti4+.Moreover,the afterglow time of Y2O2S:Eu3+,Mg2+,Ti4+nanorods can last up to1h.We pro-pose that introduction of the Mg2+and Ti4+ions to the Y2O2S compound causes the formation of new electronic donating and accepting levels between the host lattice band gap.One of the two kinds of ions absorbs energy and ther-mally transfers the excited electrons to the other kind of ions which serves as trap centers.The trapping of excited elec-trons and thermally released processes results in the after-glow.3ConclusionsSingle crystalline Y2O2S:Eu3+,Mg2+,Ti4+nanorods were prepared by solvothermal method.Results showed that the final nanorods with uniform size and smooth surface inher-ited the rod-like shape from the precursor even after calcined S W with Mg2+and Ti4+ions,the phosphorescence lasted for1h in the light perception of the naked human eye.The intro-duction of Mg2+and Ti4+ions produced the complex hole and electron traps and resulted in long-lasting phenomenon. References:[1]Lin Y H,Tang Z L,Zhang Z T,Nan C W.Anomalous lumi-nescence in Sr4Al14O25:Eu,Dy phosphors.A pplied Physics Letter,2002,81:996.[2]Jia D,Wang X,Jia W,Yen W M.Persistent energy transfer inCaAl2O4:Tb3+,Ce3+.Journal of A pplied Physics,2003,93: 148.[3]Kamada M,Murakami J,Ohno N.Excitation spectra of a long-persistent phosphor SrAl2O4:Eu,Dy in vacuum ultraviolet region.Journal of Luminescence,2000,87-89:1042.[4]Wang X X,Zhang Z T,Tang Z L,Lin Y H.Characterizationand properties of a red and orange Y2O2S-based long afterglow phosphor.Materials Chemistry and Physics,2003, 80:1.[5]Wang Y H,Wang Z L.Characterization of Y2O2S:Eu3+,Mg2+,Ti4+long-lasting phosphor synthesized by flux method.Jour-nal ofRare Earths,2006,24(1):25.[6]Wang X,Zhang J,Peng Q,Li Y D.A general strategy fornanocrystal synthesis.Nature,2005,437:121.[7]Xia Y N,Yang P D.Chemistry and Physics of Nanowires.A dvanced Materials,2003,15:351.[8]Bockrath M,Liang W J,Bozovic D,Hafner J H,Lieber C M,Tinkham M,Park H K.Resonant electron scattering by de-fects in single-walled carbon nanotube.Science,2001,291: 283.[9]Hu J T,Odom T W,Lieber C M.Chemistry and physics inone dimension:synthesis and properties of nanowires and nanotubes.A ccounts of Chemical Research,1999,32:435. [10]Wang X,Li Y D.Synthesis and characterization of lanthanidehydroxide single-crystal nanowires.A ngew andte Chemie In-ternational Edition,2002,41:4790.[11]Wang X,Sun M,Yu D P.Rare earth compound nanotubes.at C2atmosphere at high temperatures.hile co-dopedLI Wenyu et al.,Synthesis and characterization of Y2O2S:Eu3+,Mg2+,Ti4+nanorods via a solvothermal routine899Advanced Materials,2003,15:1442.[12]Yang X F,Ning G L,Lin Y.Preparation of Eu(OH)3andEu2O3Nanorods through a Simple Method.Chemistry Letters, 2007,36:468.[13]Mao Y B,Huang J Y,Ostroumov R,Wang K L,Chang J P.Synthesis and luminescence properties of erbium-doped Y2O3 nanotubes.Journal of Physical Chemistry C,2008,112:2278.[14]Jiang Y,Wu Y,Xie Y,Qian Y T.Synthesis and characteriza-tion of nanocrystalline lanthanide oxysulfide via a La(OH)3 gel solvothermal route.Journal of the A merican Ceramic So-ciety,2000,83:2628.[15]Mao S P,Liu Q,Gu M,Mao D L,Chang C K.Long lastingphosphorescence of Gd2O2S:Eu,Ti,Mg nanorods via a hydro-thermal routine.Journal ofAlloys and Compounds,2008,468: 367.[16]Zhao F,Yuan M,Zhang W,Gao S.Monodisperse lanthanideoxysulfide nanocrystals.Journal of A merican Society,2006, 128:11758.[17]Huang Y Z,Chen L,Wu L M.Crystalline nanowires of Ln2O2S,Ln2O2S2,LnS2(Ln=La,Nd),and La2O2S:Eu3+conversions via the boron-sulfur method that preserve shape.Crystal Growth &Design,2008,8:739.[18]Li W Y,Liu Y L,Ai P F.Synthesis of nanocrystalline Y2O2S:Eu3+,Mg,Ti long-lasting phosphorescent materials by hydro-thermal-microwave method.Chinese Journal of Inorganic Chemistry,2008,24:772.。
有关介孔材料的牛人课题组信息及相关文献有关介孔材料的牛人课题组信息及相关文献A mesoporous material is a material containing pores with diameters between 2 and 50 nm. Porous materials are classified into several kinds by their size. According to IUPAC notation (see J. Rouquerol et al., Pure & Appl. Chem, 66 (1994) 1739-1758), microporous materials have pore diameters of less than 2 nm and macroporous materials have pore diameters of greater than 50 nm; the mesoporous category thus lies in the middle.Typical mesoporous materials include some kinds of silica and alumina that have similarly-sized fine mesopores. Mesoporous oxides of niobium, tantalum, titanium, zirconium, cerium and tin have also been reported. According to the IUPAC notation, a mesoporous material can be disordered or ordered in a mesostructure.The first mesoporous material, with a long range order, was synthesized in the late 80s/ early 90s, by a research group of the former Mobil Oil Company (see Kresge et al., Nature 359 (1992) 710). Since then, research in this field has steadily grown. Notable examples of prospective applications are catalysis, sorption, gas sensing, optics, and photovoltaics.1. 介孔材料的诞生--1992年MS41系列分子筛(典型的是MCM-41,MCM-48,MCM-50)的合成(严格来讲,应该是1991年日本人合成出来):Nature. 1992, 359, 710-712(J. S. Beck)J Am Chem Soc. 1992, 114: 10834-10843(J. S. Beck)Science. 1993, 261: 1299-1303(霍启升)2.介孔材料制备的另一里程碑--1998年赵东元合成了SBA-15Science. 1998, 279: 548-552(赵东元)J. Am. Chem. Soc. 1998, 120, 6024-6036 (赵东元)3.通过硬模板法合成炭基介孔材料,也是一大重要成绩--1999年由韩国人刘龙完成:J Am Chem Soc. 2002, 124: 1156-1157( Ryoo R.)介孔相关的几个牛人的课题组:/doc/404424603.html,/mrl/info/publication s/(G. D. Stucky)/doc/404424603.html,/~pinnweb/(Thomas J. Pinnavaia)/doc/404424603.html,/staff/GAO/flashed/ menu.htm(Ozin's group)/doc/404424603.html,/~dyzhao/(赵东元)http://rryoo.kaist.ac.kr/pub.html (韩国刘龙(R. Ryoo))/doc/404424603.html,.sg/~chezxs/ ... n.htm (新加坡赵修松Xiusong Zhao)http://www.ucm.es/info/inorg/inv ... iones/2001/2001.htm (西班牙M. Vallet-Regi 首先把介孔材料应用到药物缓释)因为以前不小心把自己的收藏夹弄没了,所以有还有几个课题组现在没有了链接,但是其课题负责人还是记得:台湾的牟中原和他的弟子林弘平;上海硅所的施剑林;吉林大学的肖丰收和裘式伦;大化所的包信和(涉及得不多)推荐几篇介孔材料重要的综述:Chem. Mater. 1996, 8, 1147-1160 Surfactant Control of Phases in the Synthesis of Mesoporous Silica-Based Materials(Stucky和霍启升表面活性剂的堆积参数和结构的关系)Chem. Rev. 1997, 97, 2373-2419 From Microporous to Mesoporous Molecular Sieve Materials and Their Use in Catalysis (主要介绍介孔作催化载体的应用)Chem. Rev. 2006, 106, 3790-3812 Advances in the Synthesis and Catalytic Applications of Organosulfonic-FunctionalizedMesostructured Materials(有机官能化介孔的合成及在催化中的应用)Acc. Chem. Res. 2002, 35, 927-935Structural and Morphological Control of Cationic Surfactant-T emplated Mesoporous Silica(牟中原具体谈论介孔形貌的形成)Angew. Chem. Int. Ed. 2006, 45, 3216–3251 Silica-Based Mesoporous Organic-Inorganic Hybrid Materials(Frank Hoffmann 所著,非常好)Acc.Chem.Res.2005, 38,305-312 Past, Present, and Future of Periodic Mesoporous Organosilicas-The PMOs(O'zin 重点介绍周期性介孔)NATURE 2002 417 813 Ordered porous materials for emergeing application(大牛Davis所著)Chem. Mater. 1999, 11, 2633-2656 Tailored Porous Materials(Thomas J.)介孔分子筛的应用:介孔分子筛吸附氨基酸:Carbon 44 (2006) 530–536 Adsorption of L-histidine over mesoporous carbon molecular sieves(印度人A. Vinu)Separation and Purification Technology 48 (2006) 197–201 Amino acid adsorption onto mesoporous silica molecular sieves (首篇)介孔分子筛吸附蛋白质(酶)Journal of Molecular Catalysis B-Enzymatic 2(1996) 115- 126 Enzyme immobilization in MCM-4 1 molecular sieve(首篇)J. Am. Chem. Soc. 1999, 121, 9897-9898 Mesoporous Silicate Sequestration and Release of Proteins(stucky)J. AM. CHEM. SOC. 2004, 126, 12224-12225 Protein Encapsulation in Mesoporous Silicate-The Effects of Confinementon Protein Stability, Hydration, and Volumetric Properties J. Phys. Chem. B 2003, 107, 8297-8299 Adsorption of Cytochrome C on New Mesoporous Carbon Molecular Sieves(Vinu, A)介孔分子筛负载催化剂J. Phys. Chem. B 2006, 110, 15212-15217 Fabrication and characterization of mesoporous Co3O4 core-mesoporous silica shell nanocomposites(典型的core-shell结构)CHEM. COMMUN., 2003, 1522–1523 Ultra-thin porous silica coated silver–platinum alloy nano-particle as a new catalyst precursorApplied Catalysis A General 308 (2006) 19–30 Carbon oxide hydrogenation over silica-supported iron-based catalysts Influence of the preparation routeChem. Commun., 2005, 348–350 Metallic Ni nanoparticles confined in hexagonally ordered mesoporous silica material 介孔分子筛在药物可控释放方面的应用Chem. Mater. 2001, 13, 308-311 A New Property of MCM-41, Drug Delivery System (Vallet-Regi 首篇)Nature 2003, 421, 350 –353Photocontrolled reversible release of guest molecules from coumarinmodified modified mesoporous silica(第一次只能化)J. AM. CHEM. SOC. 2005, 127, 8916-8917 Fabrication of Uniform Magnetic Nanocomposite Spheres with a Magnetic Core-Mesoporous Silica Shell Structure-support(施剑林所谓的“药物分子运输车”)Angew. Chem. Int. Ed. 2005, 44, 5038 –5044 Stimuli-Responsive Controlled-Release Delivery System Based on Mesoporous Silica Nanorods Capped with Magnetic Nanopartic les(Victor S.-Y. Lin* 在智能介孔药物释放方面是贡献巨大)介孔分子筛吸附废水阳离子Chemosphere 59 (2005) 779–786 Heavy metals removal from electroplating wastewater by aminopropyl-Si MCM-41 Environ. Sci. Technol.2000, 34,4822-4827 Surfactant-Templated Mesoporous Silicate Materials as Sorbents for Organic Pollutants in WaterInd. Eng. Chem. Res. 2004, 43, 1478-1484 Highly Selective Adsorption of Pt2+ and Pd2+ Using Thiol-Functionalized Mesoporous Silica介孔分子筛在色谱中的应用Chem. Commun., 2002, 752 - 753Biomolecule separation using large pore mesoporous SBA-15 as a substrate in high performance liquid chromatographyElectrophoresis 2006,27,742–748 Large-pore mesoporous SBA-15silica particles with submicrometer size as stationary phases for high-speed CEC seperation介孔分子筛作为硬模板Adv. Mater. 2001, 13,677-681Ordered Mesoporous Carbons (Ryong Ryoo)Microporous and Mesoporous Materials 63 (2003) 1–9 Synthesis and characterization of spherical carbon and polymer capsules with hollow macroporous core and mesoporous shell structures介孔分子筛复合材料(实现光学性能,比如掺入二氧化钛,量子点)J. Phys. Chem. B 2005, 109, 12309-12315 Synthesis and Characterization of Nano titania Particles Embedded in Mesoporous Silica with Both High Photocatalytic Activity and Adsorption CapabilityChem. Mater. 2005, 17, 1269-1271 Preparation of Mesoporous Titania Thin Films with Remarkably High ThermalStabilityJ. AM. CHEM. SOC. 2006, 128, 688-689Magnetic Fluorescent Delivery Vehicle Using Uniform Mesoporous Silica Spheres Embedded with Monodisperse Magnetic and Semiconductor Nanocrystals。
第45卷第6期2006年6月Vol. 45, No. 6Jun. 2006农药Agrochemicals高纯度戊唑醇的合成与表征王 宇1,2,胡艾希1,3,陈 平4,陈 明2,刘智凌2(1.湖南大学 化学化工学院,长沙 410082;2.湖南化工研究院 精细所,长沙 410007;3.华南理工大学 化工与能源学院,广东省绿色化学产品技术重点实验室,广州 510640;4.长沙理工大学 化学系,长沙 410000)摘要:以对氯苯甲醛为原料,经缩合、加氢、环氧化、开环合成高纯度杀菌剂戊唑醇。
此工艺选择了一种新颖的催化剂避免了副产物-4,4-二甲基-3-(4H-1,2,4-三唑-4-基甲基)-1-(4-氯苯基)-3-戊醇的产生,戊唑醇总收率≥65%,不需重结晶产品纯度≥98.0%。
各项经济技术指标均超过文献水平,已工业化生产。
关键词:戊唑醇;环氧化;催化剂;合成中图分类号:TQ460.3 文献标识码:A 文章编号:1006-0413(2006)06-0397-02Synthesis and characterization of high purity tebuconazoleWANG Yu 1,2, HU Ai-xi 1,3, CHEN Ping 4, CHEN Ming 2, LIU Zhi-ling 2(1.College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, China; 2.Department of Fine Chemistry,Hunan Research Institute of Chemical Industry, Changsha 410007, China; 3.The School of Chemical & Energy Engineering, South China University of Technology, Guangzhou 510640, China; 4.Department of Chemistry,Changsha University of Science and Technology, Changsha 410000, China)Abstract: Using 4-chloropheny1aldehyde as the starting material, tebuconazole was synthesized by condensation,hydrogenation, epoxidation, and ring-opening. A new catalyst was used to avoid production of the byproduct, 4,4-dimethyl-3-(4H -1,2,4-triazole-4-ylmethyl)-1-(4-chlorophenyl)-3-pentanol. Overall yield was over 65%, and purity was over 98.0% without requiring recrystallization. Economic and technical indices of this synthetic method are more favorable than those previously reported, and the method has already been commercialized.Key words: tebuconazole; epoxidation; catalyst; synthesis戊唑醇(4,4-二甲基-3-(1H-1,2,4-三唑-1-基甲基)-1-(4-氯苯基)-3-戊醇,1)是德国拜耳公司开发的三唑类低毒高效杀菌剂[1-3],是甾醇脱甲基化抑制剂,用于重要经济作物的种子处理或叶面喷洒。
2005年第13卷合成化学Vol .13,2005 第5期,486~488Chinese Journal of Synthetic Che m istry No .5,486~488 ・快递论文・Synthtsis of Bis 2(tri a m i n oguan i di n i u m )25,5′2azotetrazol ate 3XU Song 2ling, Y ANG Shi 2qing, Y UE Shou 2ti(College of Aer onautic and Material Engineering,Nati onal University of Defense Technol ogy,Changsha 410073,China )Abstract:The synthesis of high 2nitr ogen energetic materials bis 2(tria m inoguanidinium )25,5′2az otet 2raz olate (T AGZT )fr om starting material 52a m inotetraz ole (52AT )by a novel method only in t w o step s was investigated .(1)Sodium 25,5′2az otetraz olate pentahydrate (SZT ・5H 2O )was synthesized by oxidizing 52AT with potassiu m per manganate in 15%aqueous s odium hydr oxide in yield of 75.6%.(2)The cati on rep lace ment bet w een SZT ・5H 2O and tria m inoguanidinium nitrate (T AG N )gave T AGZT,with the yield of 73.3%(m.p.196℃~197℃).The structure of T AGZT crystalwas char 2acterized by 1H NMR and 13C NMR,FT 2I R and ele mental analysis .Keywords:az otetraz olate;a m inotetraz ole;tria m inoguanidinium nitrate;synthesis;characterizati on;high 2nitr ogen energetic materialsCLC nu m ber:O626.28D ocu m en t code:A Paper nu m ber:100521511(2005)0520486203偶氮四唑三氨基胍盐的合成徐松林,阳世清,岳守体(国防科技大学航天与材料工程学院,湖南长沙 410073)摘要:以52氨基四唑(52AT )为起始原料经过两步反应合成了偶氮四唑类高氮含能化合物———偶氮四唑三氨基胍盐(T AGZT )。
Synthesis and Characterization ofNovel Polymers在化学领域,合成和表征新型高分子是一个重要的研究方向。
随着材料科学和纳米科技的发展,人们对于高分子在不同领域的应用需求越来越大,所以不断开发新型高分子材料显得尤为重要。
本文将介绍合成和表征新型高分子的研究现状和方法。
一、高分子的合成方法高分子是由大量重复单元构成的多聚物,它们的合成可以采用不同的方法,如步骤聚合法、自由基聚合法、阴离子聚合法、阳离子聚合法以及开环聚合法等。
其中,自由基聚合法是最常用的方法之一。
自由基聚合法是将引发剂加入含有单体的反应体系中,引发剂被热激活或光激活后会生成自由基,自由基会引发单体之间的反应,从而形成高分子。
这种方法可以用于合成各种不同结构的高分子,例如线性、支化、交联、复杂网络结构等。
此外,这种方法具有多样性、灵活性和高效性等优点,可以迅速制备出大规模高质量的高分子。
二、高分子的表征方法高分子的表征是确定其结构、形态和性质的过程,其结果对于研究高分子材料的应用具有重大意义。
目前,有许多技术可用于高分子的表征,其中常用的有核磁共振(NMR)、光散射(LS)、透射电子显微镜(TEM)、紫外可见光谱(UV-Vis)等。
核磁共振是一种常用的表征高分子结构的方法,它通过测量高分子中的质子、碳等原子处的共振频率和信号强度等来分析高分子的结构信息,例如单体的化学结构、聚合度、侧链化学结构等。
光散射是用于测量高分子分子量及分子量分布的方法,它可以确定高分子颗粒的大小和形状等,掌握高分子的尺寸和分子量分布等信息对于研究高分子的性能和应用非常关键。
透射电子显微镜是一种直接观察高分子形态、尺寸和结构的方法,其优点在于能够采集高分子的微观形貌信息。
然而,由于该方法需要真空条件下进行观察,因此只适用于不能发生反应的高分子样品,因为在高真空情况下高分子很容易分解。
紫外可见光谱是通过读取高分子中吸收特定波长光线的能力来分析高分子的结构和成分的方法。