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Properties of Zirconia Nanotube Arrays Loading Phospotungtic Acid

Author: LuChangYun
Tutor: ZhaoJianLing
School: Hebei University of Technology
Course: Materials Physics and Chemistry
Keywords: anodization ZrO2 nanotubes phosphotungstic acid catalyst esterification
CLC: O614.412
Type: Master's thesis
Year: 2011
Downloads: 34
Quote: 0
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Abstract


In this paper, the zirconia nanotube arrays were synthesized in organic solution byelectrochemical anodization. SEM, TEM，XRD，FTIR investigations were carried out to showthe morphology, microstructure and characteristics of the nanotubes. Then we preparedH3PW/ZrO2 catalysts. The catalyst were characterized, and used in the esterificationexperiments.1. ZrO2 nanotube arrays were prepared in organic electrolyte containing F- by anodization.A series of experiments showed that highly self-organized ZrO2 nanotube arrays can be formedin organic electrolyte of formamide and glycerol （volume-ratio 1:1） containing 1.0 wt % NH4F.These nanotubes also showed smooth and straight walls, homogeneous pipe diameter and longlength. Then, the formation mechanism of the ZrO2 nanotube arrays was discussed. Besides,ZrO2 nanotubes were optimized by different treatment technologies.2. The best catalyst preparation process was proposed as follows: using ZrO2 nanotubesannealed at 400℃as support, phosphotungstic acid （load of 35%） as active center; ZrO2 wasimpregnated in ethanol solution containing phosphotungstic acid, and then dried the samples at100℃; at last H3PW/ZrO2 was calcined in muffle furance for 4 h at 200℃in air atmosphere.3. The optimum synthesis conditions of ethyl oleate were given: the molar ratio of ethanolto oleic acid was 6:1, the dosage of catalyst was 5 mass%, the reaction time was 4 h. Finalconversion rate can reach 86.27%. The optimum conditions of synthesis of ethyl laurate were:the molar ratio of ethanol to lauric acid was 5:1, catalyst amount was 4 mass%, and the reactiontime was 4 h. The most favorable esterification reaction parameters of ethanol and stearic acidwere: ethanol and stearic acid mole was 6:1; catalyst dosage of 5 mass%, reaction time is 4h aswell.

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CLC: > Mathematical sciences and chemical > Chemistry > Inorganic Chemistry > Metal elements and their compounds > Section Ⅳ group metal elements and their compounds > The titanium Vice family ( IV B group metal elements) > Zirconium Zr
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