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用TG/DTG/DTA研究硅沸石与有机分子的主体/客体相互作用 总被引:1,自引:0,他引:1
用TG/DTG/DTA法研究无阳离子与Si—OH缺陷、结构完美的硅沸石上烃类、烷基醇、烷基胺的热脱附行为.有机分子从硅沸石上脱附的温度低于300℃其亲和性值A_T=T_d-T_b,式中T_d为有机分子在DTG上的失重峰温,T_b为该有机物在标准压力下的沸点.饱和烷烃的A_T值为60~90,而苯、甲苯、对二甲苯等的A_T值为6~13.电负性较强的羟基使烷基醇与硅沸石的亲和性明显下降.多羟基醇的A_T值为负值.对二甲苯、烷基醇、烷基胺在脱附时有明显吸热效应.A_T值及脱附热效应的不同是硅沸石骨架0~(2-)微孔表面与有机分子C—H基因,其它极性基因之间相互作用不同,以及受到硅沸石骨架空间限制的被吸附分子间缔合情况不同所致,反应了不同类型的主体/客体超分子相互作用. 相似文献
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高硅FAU沸石与甲胺吸附物的相互作用 总被引:1,自引:0,他引:1
合成高硅沸石中所用的模板剂胺类分子与沸石骨架 Si—O基团间的相互作用机理尚不清楚 .迄今为止 ,沸石与吸附胺之间的相互作用的研究还只限于测定沸石酸性质 [1,2 ]、表面羟基活性位或了解模板分子在沸石骨架中的位置和状态 [3,4 ] .甲胺、乙胺在骨架完美的高硅 FAU(Y型 )沸石上的亲和性指数 AT 值 ,即被吸附有机物脱附峰温与该有机物的沸点之差分别高达 1 60与 1 5 0℃[5] .而在高硅 MFI(Silicalite-1 )沸石上为 1 60与 1 2 7℃ [6 ] .与大多数有机物不同 ,被吸附的胺类脱附时的吸热效应十分明显 .上述现象表明胺与高硅沸石骨架 O2 -… 相似文献
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用测定吸附等温线法研究乙胺、正戊烷和乙醇在疏水高硅FAU沸石上的吸附热效应。根据Clapeyron-Clausius方程,处理吸附等温线,得到不同覆盖度C(C=被吸附分子数/晶胞)的等量吸附热Qst(C)(一定覆盖度C时由Clapeyron-Clausius方程计算的吸附热)及平均等量吸附热Qst^*(一定温度区间里等量吸附热Qst的平均值),以及Qst^*与沸点蒸发热△Hv的差值△H1(定义为相互作用强度△H1=Qst^*-△Hv)。所研究的三种有机分子的△H1的次序为△H1(乙胺)>△H1(正戊烷)>>△H1(乙醇)。这与AT值(定义为脱附温度Td与吸附质的沸点温度Tb的差值,无需单位)有正相关关系。由AT值观察到的高硅FAU沸石Si-O骨架与被吸附乙胺之间可能存在的强相互作用、为本研究测定的热力学定量数据△H1值所证明。 相似文献
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以甲胺水溶液为改性剂, 高硅Y型沸石可在常温下吸附甲胺(MA)制备有机-无机杂化酸碱双功能高硅Y型沸石材料. X 射线粉末衍射(XRD), 固体29Si魔角核磁共振(13C及29Si MAS NMR)表征表明甲胺分子与高硅Y型沸石骨架相互作用导致沸石结构发生变化, 骨架上生成新的Si—N键及Si—OH. 以热重分析(TG/DTG), NH3, CO2程序升温脱附(NH3-TPD和CO2-TPD)研究杂化Y型沸石的酸碱性质及其经不同温度焙烧后的变化, 结果表明, 杂化后沸石的酸/碱量, 尤其是后者明显增大, 其原因是骨架上生成了新的Si—OH及Si—N键. 相似文献
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化学液相沉积法调变沸石孔径及异构体择形分离 总被引:4,自引:0,他引:4
本文用化学液相沉积方法精细调变NaY沸石孔径, 在适当的溶剂中硅酯与沸石吸附水或表面羟基作用而沉积于沸石外表面, 沸石孔口有效地被缩小。制备了一系列氧化硅沉积量不同的SiNaY沸石, 红外光谱、比表面和孔体积测量结果表明随着沉积量增加沸石孔径逐渐缩小, 但沸石骨架结构、孔容和内表面性质基本不变。测定了SiNaY样品对于对二甲苯/1, 3, 5-三甲苯, β-甲基萘/α-甲基萘, 1, 2, 4-三甲苯/1, 3, 5-三甲苯, 对二甲苯/间二甲苯和对甲酚/间甲酚五类分子尺寸不同的液体混合体系的择形吸附行为, 发现SiNaY沸石对分子尺寸与沸石孔径相近的混合体系具有良好的择形选择吸附分离性能。 相似文献
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YINGCAI LONG YAOJUN SUN HONG ZENG ZI GAO TAILIU WU LIPING WANG 《Journal of inclusion phenomena and macrocyclic chemistry》1997,28(1):1-15
High resolution 29Si MAS NMR, 13C CPMAS NMR, and TG/DTG/DTA were used to study the interaction between theframework of siliceous MFI type zeolite (silicalite) and the adsorbedp-xylene. The zeolite sample used in this study possesses a perfectframework. A series of high resolution 29Si MAS NMR and 13CCP MAS NMR spectra of the samples with various loadings of p-xylene weremeasured. Experimental results of XRD, NMR and thermal analysis confirm theformation of two types of p-xylene/silicalite associate. The properties ofthe two types of associates are given in terms of their XRD patterns,NMR spectra and TG/DTG/DTA curves. When the p-xylene loading is lessthan four molecules per unit cell, the adsorbed molecules disperse inthe sinusoidal channels and interact with the framework O2-forming associate-I (p-xylene/silicalite), and inducing themonoclinic/orthorhombic(I) transition. When the p-xylene loadingis more than 5.2 molecules/u.c., the adsorbed p-xylene moleculesare located in the channel intersections and combined into ap-xylene/p-xylene complex via hydrogen bonding, formingassociate-II (p-xylene/p-xylene/silicalite) and inducingthe orthorhombic(I)/orthorhombic(II) transition. The desorptionof p-xylene from associate-II occurs at about 90 °Cwith an evident endothermic effect, whereas the desorption fromassociate-I occurs at about 140 °C without any visibleheat effect, implying that two types of sorption and desorptionprocesses exist in this host/guest system. 相似文献
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MFI沸石上对二甲苯的热脱附 总被引:4,自引:0,他引:4
MFI沸石(ZS-5型)的骨架结构内含十氧元环的二维孔道[‘],孔容积0.18cm‘·g-‘,硅沸石(Silicallte-1)是骨架中不合铝的ZSM-5.’‘StMASNMR话可揭示沸石的结构对称性、硅铝比和局部缺陷[习.Nagy等人间提出St-OH缺陷在含铅量高时形成.Woolery等门则认为出OH完全是由于骨架内包藏的桂的存在而产生,并随铝合量降低而增大.ZSM-5、硅沸石的结构特征和对二甲苯(Px)的性质决定了Px在ZSM-5上的吸附特性·本文用’‘StMASNLDEL表征硅沸石及不同含铅量的H、Na型ZSM-5的结构,并用*W**G巾TA分析吸附于… 相似文献
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环戊烷和环己烷在silicalite-1分子筛上的热脱附行为 总被引:1,自引:0,他引:1
采用智能质量分析仪(IGA)及TG/DTG法研究了环戊烷和环己烷在硅沸石silicalite-1上的热脱附行为。当环戊烷在silicalite-1上吸附量小于4 m/uc时,TG/DTG曲线表明环戊烷在silicalite-1上存在一个脱附过程。吸附量大于4 m/uc,TG曲线显示热脱附过程明显分为两个阶段,DTG曲线中出现两个明显的脱附峰,彼此分离。环己烷在silicalite-1上只存在一种脱附过程,DTG曲线只出现一个脱附峰。从环戊烷和环己烷的热脱附曲线中也可看出,随着吸附量的增加脱附峰温逐渐向高温方向偏移。 相似文献
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Aluminum Nitride Oxidation by Simultaneous TG and DTA 总被引:1,自引:0,他引:1
Dweck J. Aderne R. S. Shanefield D. J. 《Journal of Thermal Analysis and Calorimetry》2001,64(3):1163-1169
This work is a study, by simultaneous thermogravimetry (TG) and differential thermal analysis (DTA), of the oxidation of a
water resistant aluminum nitride powder which has a special protective coating, and an uncoated AlN powder which has become
partially hydrated during its use. The activation energy for oxidation is estimated by the Kissinger and isoconversional methods.
In the former method, the temperatures of the oxidation peaks were obtained from DTA and DTG curves. The activation energies
for oxidation of the water resistant AlN, obtained by the Kissinger method, are 357±10 kJ mol–1, 392±12 kJ mol–1 using respectively DTG and DTA data. For the uncoated AlN, the values are 243±7 and 257±8 kJ mol–1, respectively. By the isoconversional method, the average values obtained for coated and uncoated samples are, respectively,
323±10 and 224±7 kJ mol–1. Therefore, the special coating, which protects the aluminum nitride from humidity action, also provides a higher resistance
to oxidation.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
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This research comprises the applicability of complex thermal analysis technique (TG/DTG, DTA) in the determination of calorific
values of coals of different origin. The calorific values, those obtained by thermal analysis are compared with an adiabatic
bomb calorimeter by the standard ASTM method, and the results are discussed.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
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Šubrt J. Balek V. Criado J. M. Pérez-Maqueda L. A. Večerníková Eva 《Journal of Thermal Analysis and Calorimetry》1998,53(2):509-517
Effects induced by grinding in synthetic goethite samples were studied. The products of α-FeOOH grinding were characterised
by means of DTA, TG/DTG coupled with EGA (Mass spectrometry detection), powder X-ray diffraction analysis, and surface area
determination.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
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Water desorption from NaMgA zeolites was investigated as a function of magnesium ion content with the help of thermal analytical methods such as combined TG-DTG-DTA, TMA and X-ray heating technique. At least five partly overlapping desorption effects of water were observed from DTA and DTG features. The amount of water corresponding to individual desorption peaks was determined by experimental methods of separation. An assignment of the desorption effects to the related adsorbed forms of water is suggested. 相似文献
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The oxidation of metal sulphides and sulphide concentrates was studied by means of DTA, TG and DTG curves. The behaviour of
ZnS, CdS, GaS, Tl2S, Sb2S3 and Sb2S5 during thermal treatment in an oxidizing medium was investigated. The properties of these sulphides were compared and conclusions
were drawn about their probable oxidation reactions and the kind of end-products obtained. The characteristic temperatures
of the studied sulphides were determined on the basis of curves (DTA). The values obtained were used to compare the behaviour
of the sulphides during the oxidation process in a fluid bed. The results can be used to improve the technological and economic
indices in the industrial production of zinc.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献