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1.
笼形八苯基硅倍半氧烷的合成及表征   总被引:4,自引:0,他引:4  
杜建科  杨荣杰 《精细化工》2005,22(6):409-411
在控制水的滴加速度和体系温度的前提下,苯基三氯硅烷首先发生水解缩合形成苯基硅氧烷预聚体,然后在微量KOH催化剂作用下,制得八苯基硅倍半氧烷,收率大于90%。用傅立叶红外光谱、29Si核磁共振光谱、质谱、元素分析和热分析等手段,对它的结构和性质进行了表征。该物质的初始分解温度(失重5%)为436.8℃,热稳定性高。目前正在进行放大实验。  相似文献   

2.
在盐酸催化下,将γ-氨丙基三乙氧基硅烷在甲醇溶液中水解缩合,合成出笼型八聚(γ-氨丙基)硅倍半氧烷盐酸盐;并用四氢呋喃作沉淀剂将产物沉淀出来。利用红外、核磁和差热分析等对其结构和性质进行了表征,讨论了反应温度、反应时间、盐酸和四氢呋喃用量对反应产率的影响。结果表明,较佳合成工艺为:γ-氨丙基三乙氧基硅烷用量15mL,甲醇用量360mL,盐酸用量30mL,四氢呋喃用量250mL,在90℃下反应18h;产物熔点为412.65℃。  相似文献   

3.
以乙烯基三甲氧基硅烷为反应单体、甲醇为溶剂、四甲基氢氧化铵为催化剂,合成了正立方体的笼形八聚(乙烯基)硅倍半氧烷[(CH2CHSi O1.5)8]。讨论了反应温度、时间、碱的用量和乙烯基三甲氧基硅烷的浓度对成笼反应的影响。结果表明,较佳的工艺条件为:乙烯基三甲氧基硅烷与四甲基氢氧化铵的量之比为1∶3,乙烯基三甲氧基硅烷的浓度为0.0747g/mL,于室温下反应24h后再60℃下反应48h;此时产物的收率可达80%。产物分别用元素分析、FT-IR、1H NMR、13C NMR、29Si NMR进行了表征。  相似文献   

4.
以甲基三氯硅烷(CH3SiCl3)为主要原料,乙二胺为梯形控制剂,合成了聚甲基倍半硅氧烷,讨论了梯形控制剂,水解介质,催化剂,单体浓度,温度等因素对聚合物摩尔质量及结构规整性的影响,筛选出较佳的梯形控制剂和聚合条件。结果表明:nCH3SCl3:n乙二胺为1:1.1,产物收率接近90%,小解对nCH3SiCl3:nH2O为1:15产物摩尔质量大,且规整性好;水解后,若以四甲基氢氧化铵为催化剂。缩合反应温度为35℃时,若反应时间长,聚合物摩尔质量高,分布宽;反应时间短,则聚合物摩尔质量低,分布窄。若以酸作催化剂,缩合反应温度为80℃时,聚合物摩尔质量较低,分布也较窄。  相似文献   

5.
刘长军  李效东  田丰  张彦军 《现代化工》2005,25(Z1):130-132
用过氧乙酸氧化三乙烯基POSS(多面体低聚硅倍半氧烷)单体制备了POSS环氧化物,通过核磁共振和傅立叶变换红外光谱分析三乙烯基POSS环氧化前后结构的变化,研究并讨论了H2O2浓度、乙酸含量、反应温度、反应时间对三乙烯基POSS环氧化反应的影响.结果表明三乙烯基POSS环氧化的适宜条件是H2O2浓度50%(质量分数),反应温度70℃,CH3COOH与H2O2摩尔比0.51,反应时间h时.  相似文献   

6.
笼形八聚(氯甲基二甲基硅氧基)倍半硅氧烷的合成及表征   总被引:1,自引:1,他引:0  
以等量的四乙氧基硅烷Si(OC2H5)4与四甲基氢氧化铵Me4NOH在水溶液中水解缩合,选择性地形成笼形结构的八聚(四甲基铵)硅酸盐[(Me4NO)SiO1.5]8,将其再与氯甲基二甲基氯硅烷进行硅烷化反应,得到氯甲基二甲基氧基取代的八聚笼形倍半硅氧烷[(CH2ClMe2SiO)SiO1.5]8,分别用FTIR、1H NMR、和29SiNMR对目标产物进行了表征。考察了各反应条件对其产率的影响,得到最优合成条件为:温度25℃、反应时间17h、溶剂DMF、n(氯甲基二甲基氯硅烷)∶n八聚(四甲基铵)硅酸盐=60∶1,在该条件下产率可达72.3%。  相似文献   

7.
笼形八聚(二甲基硅氧基)倍半硅氧烷的合成与表征   总被引:3,自引:1,他引:2  
以四乙氧基硅烷〔Si(OEt)4〕与五水合四甲基氢氧化铵(Me4NOH.5H2O)为原料水解缩合得到笼形八聚四甲基铵硅酸盐([SiO1.5ONMe4]8),继而与二甲基氯硅烷〔HSi(CH3)2Cl〕反应,一锅法合成了笼形八聚(二甲基硅氧基)倍半硅氧烷(Q8M8H),最佳反应条件为:反应温度25℃,反应时间36 h,n〔Si(OEt)4〕∶n(Me4NOH.5H2O)∶n〔HSi(CH3)2Cl〕=1∶1∶4,产率80%。FTIR和NMR研究证明,所得产物为Q8M8H;SEM、EDS和XRD研究表明,所制备的Q8M8H具有较高的纯度和完整的晶型结构,属于单斜晶系,a=1.18 nm,b=1.52 nm,c=1.51nm,α=γ=90°,β=108°;TG表明,Q8M8H热失重5%时的温度为210℃。  相似文献   

8.
多面体低聚倍半硅氧烷(POSS)的合成与应用研究进展   总被引:5,自引:0,他引:5  
笼型倍半硅氧烷作为一种新型的有机/无机杂化材料,在近十年的研究中引起了人们的极大关注。这种材料的单体可以通过不同的合成方法获得,为材料的设计和剪裁提供了极大的便利。综述了笼型倍半硅氧烷单体的性质、结构与合成方法,对其应用作了浅述,同时对笼型倍半硅氧烷将来的发展趋势作了展望。  相似文献   

9.
综述了多面体低聚硅倍半氧烷(POSS)的结构特性和合成方法,重点介绍了同取代基、单官能度、双官能度、多官能度四类POSS的合成方法,比较了各种合成方法的优劣,展望了POKS合成研究的发展方向。  相似文献   

10.
以乙烯基三乙氧基硅烷为原料,通过控制水解聚合条件制得聚(乙烯基)硅倍半氧烷。IR光谱表征产物中形成了Si—O—Si的骨架结构,29SiNMR表征说明产物是以笼形结构为主,用GPC测得的摩尔质量接近五面体(T6)和六面体(T8)结构的笼形聚(乙烯基)硅倍半氧烷;通过对产物平均几何参数的计算,确定产物为笼形T6结构的聚(乙烯基)硅倍半氧烷。  相似文献   

11.
Titanium oxide compounds TiO, Ti2O3, and TiO2 with a considerable extent of nonstoichiometry were fabricated by pulsed laser ablation in water and characterized by X-ray/electron diffraction, X-ray photoelectron spectroscopy and electron energy loss spectroscopy. The titanium oxides were found to occur as nanoparticle aggregates with a predominant 3+ charge and amorphous microtubes when fabricated under an average power density of ca. 1 × 108 W/cm2 and 1011 W/cm2, respectively followed by dwelling in water. The crystalline colloidal particles have a relatively high content of Ti2+ and hence a lower minimum band gap of 3.4 eV in comparison with 5.2 eV for the amorphous state. The protonation on both crystalline and amorphous phase caused defects, mainly titanium rather than oxygen vacancies and charge and/or volume-compensating defects. The hydrophilic nature and presumably varied extent of undercoordination at the free surface of the amorphous lamellae accounts for their rolling as tubes at water/air and water/glass interfaces. The nonstoichiometric titania thus fabricated have potential optoelectronic and catalytic applications in UV–visible range and shed light on the Ti charge and phase behavior of titania-water binary in natural shock occurrence.  相似文献   

12.
The influence of the target material, fluence, laser wavelength, and nitrogen pressure on the synthesis of AlN nanosized powders via reactive laser ablation has been investigated. Using infrared laser radiation and fluences of ≥11 J/cm2, pure AlN nanosized powders were produced at nitrogen pressures of ≥1.3 kPa via ablation of an AlN target and ≥13.3 kPa via ablation of an aluminum target. With ultraviolet laser radiation, AlN powders could be synthesized at a lower fluence (9 J/cm2 at a pressure of 8 kPa). The mean powder size was 7.5−15 nm.  相似文献   

13.
采用聚焦脉冲激光法(PLA-IT/SFL)制备修饰纳米(ZnO-Eu2O3)/聚苯胺有机溶胶及其杂化薄膜材料。TEM显示金属氧化物粒子粒径约为15nm且其在聚苯胺中有较高的稳定性。荧光光谱表明该杂化薄膜材料在紫外光照射下发出强烈的黄光。热分析表明该杂化薄膜比导电性聚苯胺(PAN-HCSA)薄膜具有更好的热稳定性。该杂化薄膜材料可望用于电致发光领域。  相似文献   

14.
采用脉冲激光轰击(PIA-IT/SFL)法成功制得纳米碳/聚苯乙烯的苯溶胶并由此获得纳米碳/聚苯乙烯杂化薄膜材料。由重量差法求得杂化材料中纳米碳的含量分别为0.325%、0.615%、1.012%、1.478%、2.520%;透射电镜显示纳米碳呈圆球形均匀分散于聚苯乙烯的苯溶胶中,并且聚苯乙烯的浓度对形成的纳米碳的尺寸大小与形态分布有一定的影响;紫外光谱、荧光光谱和红外光谱表明纳米碳对聚苯乙烯的紫外吸收、荧光发光以及红外光谱等光谱性质均有影响;动态力学热分析证实少量的纳米碳可使聚苯乙烯的玻璃化温度明显降低;热重一差热分析和示差扫描量热分析表明纳米碳使聚苯乙烯的热稳定性有所提高。  相似文献   

15.
以乙烯基三乙氧基硅烷(VTES)为原料,盐酸为催化剂,经水解缩合反应合成了八乙烯基笼型倍半硅氧烷(OVS)。考察并讨论了反应温度和投料比对产物收率的影响。较佳的工艺条件为:V(VTES)∶V(HCl)∶V(CH3OH)=10∶12∶200,25℃反应18 d,收率可达31.5%。用FTIR、29SiNMR、MS和热分析对其结构和性质进行了表征。OVS失重5%对应的温度为270℃左右,说明热稳定性很高。  相似文献   

16.
采用聚焦脉冲激光轰击处于2-硝基酚蒸气氛围中的YBCO固体靶,连续制备原位修饰纳米2-硝基酚/YB-CO乙醇溶胶,进而离心烘干获得修饰性纳米2-硝基酚/YBCO杂化材料.TEM和FRTEM显示2-硝基酚修饰YB-CO基本呈现出比较规整的形貌,结晶度较低,只有部分晶格排列比较整齐;能谱扫描结果显示修饰前后样品的Y、Ba、...  相似文献   

17.
An overview of pulsed laser-assisted methods for nanofabrication, which are currently developed in our Institute (LP3), is presented. The methods compass a variety of possibilities for material nanostructuring offered by laser–matter interactions and imply either the nanostructuring of the laser-illuminated surface itself, as in cases of direct laser ablation or laser plasma-assisted treatment of semiconductors to form light-absorbing and light-emitting nano-architectures, as well as periodic nanoarrays, or laser-assisted production of nanoclusters and their controlled growth in gaseous or liquid medium to form nanostructured films or colloidal nanoparticles. Nanomaterials synthesized by laser-assisted methods have a variety of unique properties, not reproducible by any other route, and are of importance for photovoltaics, optoelectronics, biological sensing, imaging and therapeutics.  相似文献   

18.
八(乙酰苯基)笼形倍半硅氧烷的合成及表征   总被引:3,自引:0,他引:3  
以八苯基多面低聚倍半硅氧烷(OPS)为底物,无水三氯化铝为催化剂,经傅-克酰基化反应合成了笼形八(乙酰苯基)倍半硅氧烷(OAcPS)。用红外光谱、1H、13C、29Si核磁共振、元素分析、热分析等手段,对其结构和性质进行了表征。研究并讨论了溶剂用量和投料比对反应收率的影响。较佳的合成条件为:二氯甲烷用量140mL,n(acetyl chloride)∶n(OPS)=10∶1,n(AlCl3)∶n(OPS)=2.5∶1,在0℃反应6 h,产率达70%。  相似文献   

19.
In this article we report the preparation of new arylazophosphonate‐containing polymers, poly(arylazophosphonates), via polycondensation reactions of bifunctional hydroxy functionalized arylazophosphonate‐containing monomers with isocyanate or acid chloride comonomers. The polyurethanes and polyesters were characterized by common methods such as 1H, 13C, 31P NMR, FTIR, UV/visible spectroscopy, DSC, and GPC measurements. In addition, a number of polymer structuring experiments (macro and micro experiments) by means of laser ablation with a XeCl excimer laser were performed. In macro experiments, pulse number and fluence were investigated systematically and their influence on the ablation depth was discovered. In micro experiments, structures of high quality were obtained which possess clear contours without any debris on the polymer surface. Structures in the sub micron range were created by applying a phase mask. These high quality results indicate that the poly(arylazophosphonates) are well suited materials for laser ablation structuring with XeCl excimer lasers (e.g. for microstructuring or microlithography).

SEM image of sub micro structures of polymer APU 5 generated in experiments using a phase mask (line width: 0.3–0.5 μm, trench width: 0.3–0.5 μm, fluence: 3 J/cm2).  相似文献   


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