Presentation at International Seminars of Metallurgy and Materials held by LIPI in 2019.

1. Characterization of Calcined
Badau Belitung Kaolin
WRITTEN BY :
FARID MIFTHAHUL ROZAQ
UNDER SUPERVISE OF :
DONANTA DHANESWARA
RATU ULFIATI
SRI HARJANTO

2. Outline
Introduction
Materials &
Methods
• Materials,
Kaolin
Activation,
Calcination,
Characterizati
on of Kaolin
Results &
Discussions
• FT-IR, XRD, SEM,
LoI analysis Conclusions

3. Abstract
The Characterization of Belitung Kaolin after activated with NH4Cl solution and
calcined at 300, 500 and 700oC are presented in this article. Belitung Kaolin was
activated using NH4Cl solutions with a molarity of 0.5, 1, and 2 M, and then
stirred for 24 h. After the activation, the kaolin was neutralized and dried. The
dried kaolin is calcined at 300, 500, and 700oC. These samples were
characterized using FTIR, XRD, and SEM. The loss of ignition (LoI) percentages
are also presented in this article. The results indicated that metakaolin starting
to form at 500oC. This study is needed to understand kaolin behavior before
converted into the zeolite.

4. Introduction

5. Introduction
Our work was focused on Badau Belitung kaolin which
generally has a low iron and titanium content.
Kaolin is starting to be considered for catalyst raw
material because good pore structure, ease of acid
leaching, and ease of conversion into zeolite.
Our research’s main objective : synthesize Zeolite ZSM-5
from Badau Belitung Kaolin

6. Introduction
Before synthesizing the zeolite, kaolin
characteristics needed to be understood first.
To increase Kaolin’s reactivity, it has to be
converted into metakaolin.
The making of metakaolin involved
dehydroxylation of kaolin which can be done
by calcination at minimum temperature of
550oC.
Commercial Zeolite ZSM-5

7. Materials & Methods

8. Materials

9. Materials
Kaolin from Badau, Belitung
Regency, Indonesia was used for this
study.
The most dominant compounds of
our samples are SiO2 and Al2O3.
Impurities with significantly high
concentration from our samples are
Fe2O3, K2O, TiO2, and P2O5.
NH4Cl solutions with a molarity of
0.5, 1, and 2 M were used in this
study.

10. Kaolin Activation
NH4Cl
T= 50oC, t = 24 h
75 g 200 ml
[M] =
0.5, 1, 2

11. Kaolin Activation
Neutralizing Filtering
Drying
(T=110oC,
t=2 h)

12. Calcination
The masses of the samples that were going to be
calcined were measured.
The masses were varying form 7.5-8 grams.
Each sample then placed in the crucible and calcined at
300, 500, 700, 800oC for 3 and 5 hours.
The heating rate used was 10oC/min
After the calcination processes ended, the masses of
the samples were measured again to acquire the Loss of
Ignition (LoI) data.

13. Characterization of the Kaolin
Characterization that used in this study:
◦FT-IR
◦XRD
◦SEM

14. Results and Discussions

15. FT-IR Analysis
 The graphs are displaying the effects of the
temperature and duration of the calcination.
 The disappearance of OH-, Al-O, and Si-O-Al
bands are shown at the temperature of 500oC
and 700oC.
 Si-O bands still existed in every temperature.
 The duration of the calcination did not affect
the results of the calcination.

16. FT-IR Analysis
 The graphs are displaying the effects of the
temperature of the calcination and the
molarity of the NH4Cl.
 The disappearance of OH-, Al-O, and Si-O-Al
bands are shown at the temperature of 500oC
and 700oC.
 Si-O bands still existed in every temperature.
 The molarity of NH4Cl did not affect the
results of the calcination.

17. XRD Analysis
Kaolinite still exists after
calcination at 500oC
Kaolinite peaks were not
found at temperature of 700
and 800oC.
Crystals with the highest
intensity after the
calcination are quartz.
These results were
supporting the FT-IR analysis
results where the OH-, Al-Si-
O, and Al-OH bands
disappeared, and the Si-O
bands existed.

18. SEM Analysis
Kaolinite regular shape
is plate-like as shown in
the Figure.

19. SEM Analysis
SEM images of kaolin after calcined at
500oC, 700oC, and 800oC were
supporting the XRD result.
The plate-like structure of kaolinite
was still found at 500oC, while at
700oC and 800oC, kaolinite structure
was nowhere to be seen.

20. Loss of Ignition (LoI) Analysis
Chandrasekhar (1996) stated that the average loss of ignition at 450 - 550oC is
13.8% [6].
This data is close to our loss of ignition average of calcined kaolin at 500oC,
which is 11.945%.
 The slight difference potentially caused by different degree of purity of the
samples.

21. Conclusions
Kaolin is started to transform into metakaolin at 500oC.
FT-IR analysis confirmed that Si-O bands were still existed at every temperature.
This is the reason why quartz is found in every temperature in the XRD analysis.
Kaolinite structure is still found at 500oC and completely disappeared at 700oC
as confirmed by XRD and SEM analysis.
Further investigation at the temperature range of 500-700oC is needed to
confirm the temperature when the kaolinite structure disappears completely.

22. Acknowledgements

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