EXPERIMENT 3

ALUMINA EXTRACTION FROM ZEOLIT

1. Introduction
1.1 Objective
Studying metal oxide extraction from mud and characterizing the produced
compounds by FTIR.
1.2 Theory
Much attention has recently been paid to the design and application of inorganic
membranes because of their high thermal resistance, high mechanical strength and
chemical inertness. Zeolites are of great interest as new materials for inorganic
membranes because the micropore systems of zeolites are inherent for the structure
and their pore dimensions are precisely controllable by ion-exchange and chemical
vapor deposition.
The natural mixture of minerals in the soil and rocks affects the stability because
nature will recognize its components in a natural way. The steps of mineral separation
require knowledge of the inorganic cations and their solubility and chemical reactions
necessary for chemical mineral extraction. Separation of minerals in general is not a
simple process natural rocks will contain a mixture of minerals in the form of highly
stable mixed compounds. (Surjani Rahardjo, 2013)
Aluminum is a good electrical conductor. However, Al2O3 acts as an acid oxidation
or alkaline oxidation. Oxidation with with this ability is called amphoteric
(amphoteric of the Greek word amphos, meaning both). Al2O3 insoluble in water but
exhibits its amphoteric properties through its reaction with both acidic and basic
solutions.
Al2O3(s) + 6 HCl(aq)→ 2 AlCl3(aq) + 3 H2O(l)
Base acid
AlCl3(s) + 2 NaOH(aq)+ 3 H2O(l)→ 2 Na[Al(OH)4](aq)
This amphoteric properties is signifies the point of exchange of the basic oxyadtion
to the acid oxidation in the elements of the third period. (Oxtoby, 2013)
2Al(s) + 2OH-(aq) + 2H2O → 2AlO2-(aq) + 3H2(g)
Alumina can be obtained from its hydroxide heating. The heating of this hydroxide
above 850oC produces oxides that are insoluble in both acid and base, but at heating
below 600oC is obtained oxide which is soluble in both acid and base or is
amphoteric.(Kristian,2010)
Aluminum oxide is alumina (Al2O3). Nevertheless, this simplicity is offset by the
presence of polymorphic and hydrated ingredients of a nature depending on the
conditions of manufacture. There are two forms of Al2O3 anhydrous α- Al2O3 and
γ- Al2O3. Other trivalent metals (eg Ga, Fe) form the oxides both the same
structure. Both have a densely packed order of ionine oxide but differ in their cation
arrangements. α- Al2O3 is stable at high temperatures and is also infinitely
metastable at low temperatures. Its contained in nature as corundum minerals and
can be prepared by heating γ - Al2O3 or any anhydrous oxide above 1000⁰C. γ-
Al2O3 is obtained by dehydration of the dihydrate oxide at low temperature (~
450⁰C). α- Al2O3 is hard and resistant to hydration and acid absorption. γ- Al2O3
easy to absorb water and dissolve in acid; alumina used for chromatography and the
condition set for various reactivities is γ- Al2O3.
Reaction with water
Alumina can not react simply with water and is not soluble in water. Although
alumina still contains oxide ions, but the solid lattice is too strong to react with
water. Reaction with Alumina acid contains oxide ions, so it can react with acids.
For example, alumina will act with hot aqueous chloride acid to give an aluminum
chloride solution.
Al2O3(s) + 6HCl(l) → 2AlCl3(l)+ 3H2O(l)
In this case (and similar in reaction with other acids), alumina shows the basic side
of its amphoteric properties. Reactions with Alumine bases may also exhibit acid
properties, can be seen in reaction with a base such as a sodium hydroxide solution.
Hot concentrated sodium hydroxide solution can react aluminum oxide to give a
colorless sodium 10 tetrahydrosoaluminate solution.
 Al2O3(s)+ 2NaOH(aq)+ 3H2O(l)→ 2NaAl(OH)4(aq)
(Jim Clark. 2007)

2. Methods
2.1 Equipments and Materials
Equipments - Beaker glass 50 mL, Measuring glass 10 mL, Magnetic stirrer,Hot
plate,Analytical balance, pH universal indicator, Glass funnel, Glass watches,Oven,
thermometer
Materials - Dry mud, Distilled water, NaOH, HCl, Paper filter
2.2 Scheme

weighing 2,5 grams dry mud separate the precipitation

then adding 15 mL NaOH 2M using filter paper then move
and Stirring with magnetic the filtrate into beaker glass
stirrer 30 minutes 50 mL

heat the solution (70⁰C) till Adding HCl 2M solution till pH

forming the precipitation , 8, and check it using pH
then cooling it universal

Wash the precipitate with

aquadest to a neutral
weighing the final precipitate
washwater pH, then heating
mass and analyzed with FTIR
the precipitate in oven at 110
° C to a constant weight

2.3 Procedure
• 2,5 grams dry mud weighed and 15mL NaOH 2M adde then stirred for 30 minutes. The
precipitation is separated using filter paper then the filtrate moved into beaker glass 50
mL. HCl 2M solution added till pH 8, and checked by pH universal. The solution heated
(70⁰C) till the precipitation formed , then cooling it. The precipitate washed by aquadest
 to a neutral washwater pH, then the precipitate is heated in oven at 110 ° C to a constant
weight. The final precipitation mass weighed and analyzed by FTIR.

3. Discussion and Results

3.1 Result
No Sampel Result
1. Dry mud 2,5355 grams
2. NaOH 15 mL
3. HCl 10mL
4. Al2O3 0,0074 grams

19
18

16

14 2320.98cm-1
718.09cm-1
12 787.80cm-1
%T

10
3840.03cm-1 1642.72cm-1

8 3736.35cm-1
461.55cm-1

4 1051.86cm-1
3471.01cm-1
3
4000 3500 3000 2500 2000 1500 1000 500 370
cm-1
Graphic 1 . FTIR alumina from zeolit

Name Description
___ kelompok 1 Rb Alumina
1_1_1

Peak Area/Height Results

Peak X (cm-1) Y (%T) Area (%T) Start End Base1
1 3840.03 10.57 -189.15 4000 3786.76 4000
2 3736.35 9.49 -54.74 3786.76 3720.07 3786.76
3 3471.01 4.91 2444.49 3720.07 2475.74 3720.07
4 2320.98 15.81 -53.4 2475.74 2276.47 2475.74
5 1642.72 10.49 -681.1 2276.47 1573.47 2276.47
6 1051.86 3.12 -3304.42 1573.47 838.89 1573.47
7 787.8 14.89 -176.67 838.89 761.69 838.89
8 718.09 14.64 -24.98 761.69 681.96 761.69
9 461.55 9.32 -666.18 681.96 370 681.96

Calculation
𝑚1 𝑚2
SiO2 : Al2O3 = ∶
Moles SiO2 : Al2O3 60 102
5 : 1 𝑚1 𝑚2
Mr 60 : 102 5 : 1 = ∶
60 102

2,5355−𝑥 𝑥
Massa 300 : 102 5 : 1 = : 102
60
3.2 discussion 2,5355−𝑥 102
5 : 1 = x
60 𝑥

258,621−102 𝑥
5 = 60𝑥

300x + 102x= 258,621

402x= 258,621
x= 0,6433 gram

experomental yield
% Yield = 𝑥 100%
theoritical yield
0,0074
= 𝑥 100%
0,6433

= 1,15%

3.3 Discussion

In this experiment , the mud is calcined (heating) first, the aim of this treatment to
removing water and other organic / volatile substances for 1 hours.
Mixing the mud with concentrated NaOH solution(15ml), then Al2O3 dissolved and
produces aluminate ions. Reaction :
Al2O3 + 2OH- 2AlO2- + H2O.
Stir with a magnetic stirrer. After stirring with a magnetic stirer then acidified with the
addition of HCl solution 2 M drop by drop till pH 8, check it using pH universal. In this step,
 you must be careful because the addition of HCl excess can lowered pH value and then
influenced for the next step . The reaction: AlO2- + HCl Al (OH) 3 + Cl
Then heated using hot plate with temperature 70⁰C (constant) for 30 minutes till formed the
precipitation (White precipitation). Produces:
2Al (OH) 3 Al2O3 + H2O
After that , separate the precipitation from filter using filtered paper, then wash it using aquades
to remove the impurities. And dried the precipitation witrh oven in 110 ⁰C for 2 hours. Carefully,
move the precipitation and using analytical balance weighing the drying precipitation, we get
0,0074 grams. The main impurities of sludge (bauxite) usually consist of SiO2, Fe2O3, and TiO2.
And after the calculation we can get the % yield of alumina is 1,15%
FTIR test for alumina

Using FTIR to test the alumina to know what the bonding in the compounds. Before test the
sample, FTIR must be cleaning using aceton then use plat KBr. After that, the sample test . from
the graphice of FTIR about the alumina, we know that the bonding in the alumina showed in
every peaks of the graphic.

2320,98 C-H bonding

1642,12 C-H bonding
1051,86 C-C bonding
787,80 C-C bonding
718,09 C-C bonding
461,55 C-H bonding

4. Closing
-conclusion
From the experiments about the extraction alumina from zeolite(mud) we get % yield of
Al2O3 is about 1,15% that’s mean the impurities in the sample substance is still a lot
-suggestion
Must be careful, especially when the adding of HCl to get pH 8. And always paid
attention.
5. References
- Oxtoby, D.W., H.P. Gillis and N.H. Nachtrieb, 2003. Prinsip-Prinsip Kimia Modern.
Edisi Keempat jilid II. Terjemahan S.S. Achmadi. Erlarngga, Jakarta.
- Clark, Jim. 2007. Sifat Asam-Basa dari Oksida-Oksida Periode 3. http://www.chemis-
try.org/materi_kimia/kimia_anorganik1/unsur-unsur_periode_3/
sifat_asam_basa_dari_oksida_oksida_periode_3/.
- Sugiarto, H. Kristian dan Retno D. Suyanti. 2010. Kimia Anorganik Logam. Yogyakarta:
Graha Ilmu

6. Appendix

Ph test using ph universal filtering the solution

Filtering the solution to get yield yield after heating in the oven
Weighing the yield after the addition of HCl

The precipitation