A study of m study of methods of thods of extra xtracting c ting - PowerPoint PPT Presentation

A study of m study of methods of thods of extra xtracting c ting che hemic ical produc l products from ts from oil sha oil shale le a ash sh Shucai Gan, , Haifeng Zou, Xuechun Xu, Guimei Gao Changchun, P.R.China 2010. 10. 20

Outline 1 Introduction of oil shale ash 2 Preparation of nano-sized alumina 3 Synthesis of silica nanoparticles 4 Preparation of silica aerogels College of chemistry

Ⅰ Introduction of oil shale ash • Oil shale ash (OSA) is a by-product of oil shale processing, which accounts for 60 – 70 wt. % of the raw oil shale. The OSA is rich in inorganic elements, such as aluminum and silicon, which can be used to produce chemical products by hydrometallurgical technology. College of chemistry

Ⅰ Introduction of oil shale ash • For our experiments, oil shale ash was obtained from Jilin province. The main properties of OSA are as follows: Q-quartz Q K-kaolinite X-metakaolin fs-alkali feldspar Intensity (a.u.) Pl-plagioclase Q K K Q Q Oil shale Oil shale ash X fs Q Pl Q Oil shale ash Oil shale ash 10 20 30 40 50 60 calcined 2 θ in degree College of chemistry

Ⅰ Introduction of oil shale ash Table 1 Chemical compositions of oil shale ash Component Oil shale ash (wt.%) SiO 2 51.66 Al 2 O 3 23.22 Fe 2 O 3 5.20 CaO 3.38 MgO 0.17 K 2 O 0.93 Na 2 O 0.11 College of chemistry

Outline 2 Preparation of nano-sized alumina College of chemistry

Ⅱ Preparation of nano-sized alumina • Nano-sized alumina has considerable potential for a wide range of applications such as catalysts, electronic devices, and fine ceramic composites. • In our work, nano-Al 2 O 3 was prepared from oil shale ash via an ultrasonic technique followed by azeotropic distillation. Baichao An, Shucai Gan * ,Energy,35 (2010) 45-49; Chemical Engineering Journal 157 (2010) 67–72; College of chemistry

Ⅱ Preparation of nano-sized alumina • 2.1 The synthesis flowchart Oil shale ash H 2 SO 4 Solution Residue NaOH pH =13 Sodium aluminate PEG CO 2 aluminum hydroxide nano-sized Aging, Sonication alumina azeotropic distillation College of chemistry

Ⅱ Preparation of nano-sized alumina • 2.2 The main properties of nano-size alumina 58 nm 16 nm Figure 1. XRD pattern of nano-Al 2 O 3 powders (a: α - Al 2 O 3 ; b: γ - Al 2 O 3 ) College of chemistry

Ⅱ Preparation of nano-sized alumina Figure 2. TEM micrographes of the nano-size Al 2 O 3 (a: α -Al 2 O 3 ; b: γ - Al 2 O 3 ) College of chemistry

Ⅱ Preparation of nano-sized alumina Table 2 Chemical compositions of α -Al 2 O 3 Component Alumina (wt.%) SiO 2 0.0572 Al 2 O 3 99.80 Fe 2 O 3 0.0103 CaO 0.0256 MgO 0.0021 K 2 O 0.0038 Na 2 O 0.0474 The purity of alumina reaches 99.80%, which is suitable for many applications. College of chemistry

Ⅱ Preparation of nano-sized alumina The results show that the alumina prepared by this method has a mesoporous structure and the specific surface area is as high as 152 m 2 /g with a dominant pore diameter of 14.30 nm . 140 0.25 3 /g STP) Artifact (tensile strength effect) 14.30 nm 2 /g BET Sufrace Area=152.32cm 120 0.20 Pore Volume ( cm3/g ) Quantity adsorption (cm 100 0.15 80 14.30 nm 0.10 60 0.05 40 20 0.00 0.0 0.2 0.4 0.6 0.8 1.0 1 10 100 Relative pressure ( P / Po ) Pore diameter (nm) Figure 3 N 2 adsorption-desorption isotherms and pore size distribution of the alumina powders College of chemistry

Outline 3 Synthesis of silica nanoparticles College of chemistry

Ⅲ Synthesis of silica particles 3.1 Applications of silica nanoparticles Adsorbents fine precision equipment Catalytic Humidity nano-silica supports sensors colloidal damper in the field of mechanical engineering College of chemistry

Ⅲ Synthesis of silica particles 3.2 The synthesis flowchart The resultant residue and sodium hydroxide solution was mixed, and boiled for 5 h with constant stirring to dissolve the silica and produce water glass. Guimei Gao, Shucai Gan * ,Powder Technology 202 (2010) 137–142; College of chemistry

Ⅲ Synthesis of silica particles polyethylene Water glass glycol Adding H 2 SO 4 under ultrasonic Silica gel Nano-SiO 2 Aging, filtrating Distilling College of chemistry

Ⅲ Synthesis of silica particles 3.3 The main properties of silica nanoparticles 3000 2500 Intensity (a.u.) 2000 1500 1000 500 0 10 20 30 40 50 60 70 2 θ / ° Figure 3 XRD pattern of Figure 4 TEM micrograph nano-silica of nano-silica College of chemistry

Ⅲ Synthesis of silica particles Table 2 Chemical compositions of silica powders Component Silica powders (wt.%) SiO 2 99.96 Al 2 O 3 0.01 Fe 2 O 3 0.0063 CaO 0.0031 MgO 0.0054 K 2 O 0.0031 Na 2 O 0.014 College of chemistry

Outline 4 Preparation of silica aerogels College of chemistry

Ⅳ Preparation of silica aerogels Silica aerogels are novel mesoporous materials with many desirable properties, such as low bulk density, continuous porosities, high specific surface area and so on. Silica aerogels are promising materials as super-thermal insulators, catalytic supports, adsorbents and host materials for drug delivery systems. Sketch map of aerogels College of chemistry

Ⅳ Preparation of silica aerogels 4.1 Flowchart for the synthesis Aerogels Water glass ammonia Drying Surface modification Solvent Aging exchange College of chemistry

Ⅳ Preparation of silica aerogels • 4.2 The main properties of silica aerogels Figure 2. SEM micrograph of silica aerogels Guimei Gao, Shucai Gan * , Powder Technology 191 (2009) 47; Powder Technology 197 (2010) 283; and Materials Letters 63 (2009) 2721; College of chemistry

Ⅳ Preparation of silica aerogels 1800 (d) 9 8 Quantity adsorption ( cm3/g STP ) Pore Volume ( cm3/g ) 1500 BET:980 cm 2 /g 7 6 PD:10.8nm 1200 5 4 3 900 2 1 600 0 1 10 100 Pore diameter (nm) 300 0 0.0 0.2 0.4 0.6 0.8 1.0 Relative pressure ( p/p o ) Figure 3 N 2 adsorption-desorption isotherms and pore size distribution of the silica aerogels College of chemistry

Conclusion In summary, chemical products such as nano- sized alumina, silica nanoparticles and aero- gels, have been synthesized using OSA for the first time. The developed methods could be part of a comprehensive utilization scheme for OSA. College of chemistry

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