Study on peptizability of boehmite and its application for the peparation of y-Al2O3 in spherical shape

The optimal technological parameters for the spheroidization of y-Al2O3 have been found. The obtained spheres of y-Al2O3 have various desired diameters, high mechanical strength and high surface area. It has increased the application value of y-Al2O3.

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158 Journal of Chemistry, Vol. 45 (Special issue), P. 158 - 161, 2007 STUDY ON PEPTIZABILITY OF BOEHMITE AND ITS APPLICATION FOR THE PEPARATION OF -Al2O3 IN SPHERICAL SHAPE Received 15 October 2007 Nguyen Han Long, Tran Vinh Hoang, Pham Thanh Huyen Faculty of Chemical Technology, Hanoi University of Technology summary This paper presents the results of the peptizability of boehmite and its application for the preparation of -Al2O3 in spherical shape. The obtained -Al2O3 in spherical shape has high mechanical resistance and high surface area. The water vapor adsorption ability of sphere of - Al2O3 has also been determined. -Al2O3 in spherical shape can adsorb moisture up to 65% of their weight. I - INTRODUCTION -Al2O3 is a mesoporous material which has high acidity, activity, good mechanical and thermal resistance. So -Al2O3 is widely used as the adsorbent and catalyst in the refinery and petrochemical technology in particular, and in the chemical industry in general [1, 2]. However, in order to use it in chemical processes, beside the study to increase its surface area [3], the formation of -Al2O3 in spherical shape is very important. One of the most important properties of boehmite is its peptizability to be the binder for other materials that do not have this ability. So the application of boehmite as the binder has greatly increased the value and the application range of -Al2O3 and other materials. The refinery and petrochemical industry is being built in Vietnam. Each year, a large amount of -Al2O3 in spherical shape is imported to be used as the adsorbent in the drying of natural gas. So finding a procedure to synthesize -Al2O3 in spherical shape from cheap and available domestic raw material is very necessary. II - EXPERIMENTAL -Al2O3 has been synthesized from available domestic raw materials such as waste aluminum, Tan Binh aluminum hydroxide and industrial aluminous material. Other chemicals include: NaOH, H2SO4, H2O2, organic additives and peptization reagent. These chemicals are firstly used in pure form and then in industrial form to determine the reiteration and prepare to manufacture in the large scale. The procedure to synthesize -Al2O3 and to form the finished product is shown in Fig. 1. The procedure to form the sphere of -Al2O3 is as follow: first, the viscosity of peptization solution is adjusted to a suitable value by adding distilled water, and then it is forced through holes with different sizes to form spheres with different diameters. These drops fall slowly through a column containing different layers of oil and ammonia. At the bottom, the spheres are separated, dried and calcined. The obtained boehmite and -Al2O3 are characterized by X-ray diffraction (XRD) on a 159 D8 Advance (Bruker) at Petrochemical and Catalysts Material Laboratory, Hanoi University of Technology (PCM-HUT). Analysis regime is: Cu K radiation ( = 1,5406 Å), voltage of 40 kV, electric current of 40 mA, temperature of 25oC, 2 = 10 - 70o, step 0,1o etc... III - RESULTS AND DISCUSSION 1. Characterization of obtained boehmite and -Al2O3 by XRD XRD patterns of boehmite and -Al2O3 are shown in Fig. 2. Figure 1: Procedure of the synthesis and spheroidization of  - Al2O3 Figure 2: XRD patterns of boehmite (a) and -Al2O3 (b) Fig. 2 shows that obtained boehmite and - Al2O3 contain only single phase characterized for boehmite and -Al2O3. It has confirmed that the obtained products are very pure. XRD pattern of peptization boehmite gel after drying at 120oC is exactly the same as that of boehmite. It means that peptized reagent has completely been decomposed at  120oC. 2. Influence of technological parameters on the spheroidization of -Al2O3 Through preliminary studies, it is found out that when the content of peptization reagent was greater than 10%, the obtained gel after calcination was very hard and brittle and the adsorption ability of the product was very low, so it is not suitable to be used as a binder. PCM - Bruker D8 Advance - Boehmite 88-2110 (C) - Boehmite, syn - AlO(O(H.33D.67)) - Y: 50.00 % - d x by: 1. - WL: 1.5406 - Orthorhombic - a 2 Li n (C ps ) 0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 2-Theta - Scale 10 20 30 40 50 60 70 a PCM - Bruker D8 Advance - gama Al2O3 29-1486 (D) - Aluminum Oxide - gamma-Al2O3 - Y: 83.33 % - d x by: 1. - WL: 1.5406 0 10 20 30 40 50 60 2-Theta - Scale 10 20 30 40 50 60 70 Li n (C ps ) b 160 Moreover, according to references [1, 4], the greater the peptization content, the lower the surface area of -Al2O3. With the data obtained in the studies of the influence of peptization regent content on the mechanical resistance and adsorption ability of spheres of -Al2O3, it has been realized that the content of peptization reagent is optimal between 6 - 7%. The results obtained in the spheroidization of -Al2O3 with different oil, different height of oil and ammonia column is presented in table 1. Table 1: Influence of some technological parameters on the spheroidization of -Al2O3 Column Height, mm Result Peanut oil - Bean oil - No spheres formed 10 flattish shape 20 flattish shape 30 spherical shape 40 spherical shape Kerosene 50 flattish shape 50 spheres are stuck together 70 spheres are stuck together 100 spheres are separated Ammoni a 10% 150 spheres are separated When the drops of peptized boehmite falls through oil column, under the surface tension force, these drops tend to form the spherical shape. When they fall through the ammonia column with the height greater than 100 mm, the outside layer will be neutralized, hardened. These harden drops fall to the bottom of the column and are neither distorted nor stuck together [5]. If the height of the ammonia column is less than 100 mm, the peptized boehmite drops can not be neutralized completely, so they are stuck together. So, by using the kerosene column with the height of 30 ÷40 mm and the ammonia column greater than 100 mm, we can obtain -Al2O3 in spherical shape with various diameters. With the peptized boehmite gel, extrudates can also be form by extrudation. The obtained extrudates are then dried and calcined to get the finished products. The photo of spheres and extrudates of - Al2O3 with diameter of 3mm is shown in Fig. 3. From the above results, this procedure can be applied to form the spheres and extrudates of other materials such as zeolites to be used as catalysts or adsorbents...to increase the value and the application range of these materials. 3. Study the adsorption ability of product The results that present the relationship between adsorbed moisture content/-Al2O3 weight (A%) and time on stream are shown in Fig. 4. Figure 3: Photo of spheres and extrudates of -Al2O3 161 0 5 10 15 20 25 30 0 10 20 30 40 50 60 70 M oi st ur e A ds or pt io n, A % T im e(days) Figure 4: Moisture adsorption ability of -Al2O3 in spherical shape Fig. 4 shows that spheres of -Al2O3 adsorb moisture quickly at the beginning (< 3 days), then the adsorption will slow down and reach the saturated level after 30 days with the adsorbed moisture content up to 65% of the - Al2O3 weight. These initial results prove that spheres of - Al2O3 meet the necessary requirements to be applied as the adsorbent in the drying of natural gas. CONCLUSIONS - -Al2O3 has been synthesized from cheap and available domestic raw materials. - The optimal technological parameters for the spheroidization of -Al2O3 have been found. The obtained spheres of -Al2O3 have various desired diameters, high mechanical strength and high surface area. It has increased the application value of -Al2O3. - Spheres of -Al2O3 have good adsorption ability, so they can be used in the drying of natural gas. REFERENCES 1. Bruce E. Leach. Applied industrial catalysis, Vol. 3, Academic Press (1984). 2. R. J. Farrauto and C.H. Bartholomew, Fundamentals of Industrial Catalytic Processes, Blackie Academic & Professional (1999). 3. Pham Thanh Huyen, Nguyen Han Long, Tran Vinh Hoang. Proceedings of the 4th Asia-Pacific Chemical Reaction Engineering Symposium, Gyeongju, Korea, 12-15 June 2005. 4. Tran Cong Khanh. Experiments of organic synthesis. Hanoi University of Technology, (1976). 5. James T. Richardson. Principles of catalyst development, Plenum Press, New York and London (1992).

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