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

• il sha
• il shale

le a ash sh

Shucai Gan, , Haifeng Zou, Xuechun Xu, Guimei Gao Changchun, P.R.China

• 2010. 10. 20

1

Introduction of oil shale ash

2

Preparation of nano-sized alumina

3

Synthesis of silica nanoparticles

4

Preparation of silica aerogels

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Outline

• Oil shale ash (OSA) is a by-product of
• il 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.

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ⅠIntroduction of oil shale ash

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10 20 30 40 50 60

Intensity (a.u.) 2θ in degree

Oil shale ash Oil shale K

Q

K

Q

Q Q Q X fs Pl Q

Q-quartz K-kaolinite X-metakaolin fs-alkali feldspar Pl-plagioclase

Oil shale ash Oil shale ash calcined

Ⅰ Introduction of oil shale ash

• For our experiments, oil shale ash was
• btained from Jilin province. The main

properties of OSA are as follows:

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Component Oil shale ash (wt.%) SiO2 51.66 Al2O3 23.22 Fe2O3 5.20 CaO 3.38 MgO 0.17 K2O 0.93 Na2O 0.11 Table 1 Chemical compositions of oil shale ash

Ⅰ Introduction of oil shale ash

2

Preparation of nano-sized alumina

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Outline

College of chemistry Baichao An, Shucai Gan*,Energy,35 (2010) 45-49; Chemical Engineering Journal 157 (2010) 67–72;

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-Al2O3 was prepared from
• il shale ash via an ultrasonic technique

followed by azeotropic distillation.

College of chemistry Oil shale ash Sodium aluminate

H2SO4

nano-sized alumina

pH =13 NaOH

Solution

PEG

aluminum hydroxide

CO2 Aging, Sonication azeotropic distillation

Residue

Ⅱ Preparation of nano-sized alumina

• 2.1 The synthesis flowchart

College of chemistry Figure 1. XRD pattern of nano-Al2O3 powders (a: α- Al2O3; b: γ- Al2O3)

58 nm 16 nm

Ⅱ Preparation of nano-sized alumina

• 2.2 The main properties of nano-size alumina

College of chemistry Figure 2. TEM micrographes of the nano-size Al2O3 (a: α-Al2O3; b: γ- Al2O3)

Ⅱ Preparation of nano-sized alumina

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Component Alumina (wt.%) SiO2 0.0572 Al2O3 99.80 Fe2O3 0.0103 CaO 0.0256 MgO 0.0021 K2O 0.0038 Na2O 0.0474 Table 2 Chemical compositions of α-Al2O3 The purity of alumina reaches 99.80%, which is suitable for many applications.

Ⅱ Preparation of nano-sized alumina

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0.0 0.2 0.4 0.6 0.8 1.0 20 40 60 80 100 120 140

Quantity adsorption (cm

3/g STP)

Relative pressure (P/Po)

BET Sufrace Area=152.32cm

2/g

1 10 100 0.00 0.05 0.10 0.15 0.20 0.25

Pore diameter (nm) Pore Volume ( cm3/g)

14.30 nm

Figure 3 N2 adsorption-desorption isotherms and pore size distribution of the alumina powders

14.30 nm

Artifact (tensile strength effect)

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 m2/g with a dominant pore diameter of 14.30 nm .

3

Synthesis of silica nanoparticles

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Outline

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nano-silica fine precision equipment Adsorbents Catalytic supports Humidity sensors colloidal damper in the field of mechanical engineering

Ⅲ Synthesis of silica particles

3.1 Applications of silica nanoparticles

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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;

Ⅲ Synthesis of silica particles

3.2 The synthesis flowchart

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polyethylene glycol Distilling Water glass Silica gel Aging, filtrating

Nano-SiO2 Adding H2SO4 under ultrasonic

Ⅲ Synthesis of silica particles

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10 20 30 40 50 60 70 500 1000 1500 2000 2500 3000

Intensity (a.u.) 2θ / °

Figure 4 TEM micrograph

• f nano-silica

Figure 3 XRD pattern of nano-silica

Ⅲ Synthesis of silica particles

3.3 The main properties of silica nanoparticles

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Component Silica powders (wt.%) SiO2 99.96 Al2O3 0.01 Fe2O3 0.0063 CaO 0.0031 MgO 0.0054 K2O 0.0031 Na2O 0.014 Table 2 Chemical compositions of silica powders

Ⅲ Synthesis of silica particles

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4

Preparation of silica aerogels

Outline

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Sketch map of aerogels

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.

College of chemistry ammonia Water glass Drying Aging Solvent exchange Surface modification Aerogels

Ⅳ Preparation of silica aerogels

4.1 Flowchart for the synthesis

College of chemistry 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;

Ⅳ Preparation of silica aerogels

• 4.2 The main properties of silica aerogels

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0.0 0.2 0.4 0.6 0.8 1.0 300 600 900 1200 1500 1800

1 10 100 1 2 3 4 5 6 7 8 9

Pore Volume ( cm3/g) Pore diameter (nm)

Quantity adsorption ( cm3/g STP) Relative pressure ( p/po)

(d)

Figure 3 N2 adsorption-desorption isotherms and pore size distribution of the silica aerogels

BET:980 cm2/g PD:10.8nm

Ⅳ Preparation of silica aerogels

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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

• f a comprehensive utilization scheme for OSA.

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Thanks for your attention!