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1.
王洁欣  文利雄  和平  陈建峰 《化学学报》2005,63(14):1298-1302
以纳米碳酸钙颗粒为新颖的无机模板剂, 硅酸钠为无机硅源, 通过溶胶-凝胶法形成CaCO3/SiO2的核壳结构; 随后通过高温煅烧、酸溶和干燥处理, 合成出了具有高比表面积的球形纳米空心二氧化硅粒子. 然后, 分别采用TEM, SEM, EDS, XRD, FTIR和TG等测试手段对样品进行了分析和表征, 并考察了不同合成条件, 如反应温度、反应pH值、煅烧温度和包覆反应时SiO2/CaCO3的配比对纳米空心二氧化硅粒子的比表面积变化. 实验结果表明: 较高的反应温度如60~80 ℃, pH值9左右、SiO2包覆量为碳酸钙质量的10%, 以及煅烧温度为700 ℃, 有利于形成空心形貌较好、比表面较大的球形纳米空心二氧化硅.  相似文献   

2.
采用共沉淀法制备了高钛含量的复合氧化物TiO2/SiO2.用BET、XRD、FT-IR和正胺吸附等分析手段,研究了煅烧温度对TiO2/SiO2表面酸量的影响.研究发现,随着煅烧温度的升高,TiO2/SiO2表面羟基密度、比表面积逐渐减少,TiO2晶粒尺寸变大,造成TiO2/SiO2表面酸量降低.当煅烧温度达到600℃到800℃之间,表面酸量基本不再改变.  相似文献   

3.
采用溶胶-凝胶法合成粒径在50—150nm范围内的二氧化硅(SiO2)纳米粒子。用甲基丙烯酸-3-(三甲氧基硅基)丙酯(MPS)对SiO2纳米粒子表面进行修饰,使其表面接枝能参与自由基聚合反应的碳碳双键基团。用元素分析、FTIR、^13C CP/MASNMR和^29Si CP/MASNMR等手段对修饰过的SiO2纳米粒子进行表征,以确证MPS接枝在SiO2纳米粒子上。分析修饰过的SiO2纳米粒子的^29Si CP/MASNMR和FTIR谱图,还可初步推断MPS接枝在SiO2纳米粒子表面的机理:MPS首先发生水解缩合反应形成低聚物,然后通过氢键作用吸附到SiO2纳米粒子表面,最后MPS低聚物中未缩合的硅羟基与SiO2纳米粒子表面的硅羟基发生缩合反应。  相似文献   

4.
张辉  刘莲云  安振涛  张登君  唐清 《化学学报》2005,63(12):1131-1135,i005
提出了一种工艺简单、成本低廉的准气相反应合成ZrO2球的新方法.通过对产物的SEM观测表明:该方法制备的ZrO2粒子为较好的球形,球表面光滑;其平均粒径1.71μm,标准偏差0.49um;球有三种结构:均匀敛密结构、核心疏松外层致密结构和空心结构;经600℃煅烧后,XRD分析确定ZrO2球的相组成主要为立方相.  相似文献   

5.
邹华  吴石山  沈健 《化学学报》2009,67(3):266-269
聚乙烯吡咯烷酮(PVP)功能化的聚苯乙烯(PS)粒子在SiO2包覆的同时被乙醇/氨水介质溶解, 得到了单分散空心SiO2纳米微球. 该空心SiO2纳米微球的尺寸和形态可以通过PVP, NH4OH和正硅酸乙酯(TEOS)的用量来调节. PVP用量增加导致PS粒子变小, 从而得到较小的空心SiO2纳米微球; NH4OH用量增加, 空心SiO2纳米微球表面变得粗糙; TEOS用量增加, 空心SiO2纳米微球的壳层厚度增加. 包覆(溶解)温度是控制空心SiO2纳米微球形成的最有效手段. 在70 ℃的包覆(溶解)温度下可以获得全部空心的SiO2纳米微球.  相似文献   

6.
采用Stber方法,通过调节反应温度及乙醇和水的体积,合成了不同粒径的二氧化硅纳米粒子.以合成的粒径为20nm的二氧化硅纳米粒子为原料,采用简单、方便的喷涂方法在玻璃片上构筑了纳米粒子涂层.在550℃煅烧二氧化硅纳米粒子涂层,增强了二氧化硅纳米粒子在玻璃片上的附着力.用1H,1H,2H,2H-全氟辛基三乙氧基硅烷修饰之后,二氧化硅纳米粒子涂层的表面润湿性由亲水性转变为疏水性.通过喷涂法制备的二氧化硅纳米粒子涂层具有减反增透效果,当二氧化硅纳米粒子质量分数为0.48%、循环喷涂沉积数为3时,涂层在可见光范围内的最大透光率可达95.5%.用扫描电子显微镜观测涂层表面形貌发现,喷涂法制备的涂层是均匀的、可控的.喷涂技术构筑纳米粒子涂层具有简单快速、可大面积应用等优点.  相似文献   

7.
张辉  安振涛  张登君  唐清 《化学学报》2005,63(22):2098-2102
采用新颖的准气相反应法,合成出了球形度好、表面光滑的ZrO2微球.通过对产物的SEM,TEM和XRD表征,研究了煅烧温度对ZrO2球结构特性的影响.结果表明:经600~800℃煅烧后,生长完好的ZrO2球,其显微结构为均匀多孔结构,纳米晶粒呈花生样的长条形状;ZrO2球的相由主要的立方相和少量的四方相组成.  相似文献   

8.
朱家艺  贺军辉 《化学学报》2010,68(10):961-968
通过改变反应物物质的量比、分散相与连续相体积比、反应体系温度和煅烧后处理温度,研究了反应条件对乳液法自组装合成氧化锰纳米粒子结构、形貌和尺寸的影响.结果表明:当高锰酸钾与油酸物质的量比在1∶5~1∶1之间时,形成蜂窝状纳米粒子和空心纳米粒子;当分散相(油酸)与连续相(水)的体积比为4∶200时,形成良好的空心球纳米结构;反应体系温度升高不利于产物的洗涤;不同温度的煅烧后处理不仅影响氧化锰纳米粒子的形貌,而且影响其结晶度和晶型.  相似文献   

9.
SiO_2/PVAc无机-有机复合微球的合成及其膜性能研究   总被引:1,自引:0,他引:1  
以纳米二氧化硅粒子(SiO2)为稳定剂,在少量反应型阴离子乳化剂——烯丙氧基羟丙磺酸钠(HAPS)作助稳定剂的情况下,制备了具有草莓型结构的二氧化硅/聚醋酸乙烯酯(SiO2/PVAc)无机-有机纳米复合微球.研究表明,纳米SiO2与PVAc的氢键作用是形成这种单分散草莓型SiO2/PVAc无机-有机纳米复合微球的关键.透射电镜(TEM)观察显示,纳米SiO2吸附在PVAc表面,形成草莓型结构.讨论了纳米二氧化硅溶胶的种类和用量、乳化剂种类对复合微球形态及其膜性能的影响,并讨论了复合微球的形成机理.  相似文献   

10.
PTFE/纳米SiO2复合材料的制备及其力学性能   总被引:1,自引:0,他引:1  
聚合物/纳米级无机粒子复合材料是纳米材料中的一种具有重要价值的新型材料,可广泛应用于橡胶、塑料、纤维三大合成材料之中。采用纳米级无机粒子填充聚合物基复合材料,可以在材料的补强、增韧等改性中获得良好的效果。本文以纳米SiO2为填料,将其经过有机处理后,制备了FIFE/纳米SiO2复合材料,并研究了纳米SiO2的含量对PTFE复合材料性能的影响。  相似文献   

11.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

12.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

13.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

14.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

15.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

16.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.  相似文献   

17.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

18.
19.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

20.
A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.  相似文献   

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