ABAL ABAL

Characterization of catalyst by XRD method aims to review the structure and

crystallinity of a catalyst. The result of XRD pattern of catalyst 5% K2O / CaOZnO with various ratio mol of CaO-ZnO shown in figure 1. Diffractogram of CaO
shows intensity and peak at angle 2: 17.2 , 28.7 , 50.5 , and 52.7 (JCPDS
File No. 37-1497) (Taufiq-yap et al. 2010). Meanwhile, XRD patterns of ZnO visible
at angle 2: 31.84 , 34.51 , 36.33 , 47.62 , 56.66 , 62.92 , 66.41 , 68 ,
69.13 , 76.98 and 89.67 (JCPDS File No. 36-1451) (Software Game! 3). Then,
the impregnation result of 5%W K2O upon CaO-ZnO catalyst gives additional
peak intensity at angle 2: 23.88 , 39.49 , 46.67 , 48.88 and 64.57 .
Figure 2 shows the results in accordance with the composition of the catalyst
that has been made. Diffraction for CaO and ZnO on both catalysts showed a
similar pattern, only has a peak slightly smaller due to a decrease in the content
of CaO or ZnO in the catalyst (Mutreja et al. 2014). The XRD pattern shows that
the structure and crystallinity of the catalyst with CaO-ZnO ratio of 1: 3 provides
the highest intensity of ZnO. While the intensity of the highest CaO owned by
catalysts with CaO-ZnO ratio of 3: 1. K2O diffraction showed little intensity in the
XRD pattern. The small size of the peak intensity of K2O were detected as a
result of his K2O concentrations are evenly spread over the surface of the
catalyst.
==Catalyst 5%K2O/CaO-ZnO preparation has been done with variation mole
ratio of CaO:ZnO. The catalyst then tested to determine the basicity (Tanabe,
1964). Basicity test method using titration by benzoic acid and benzene as the
solvent, using bromotymol blue (BTB) show the result that can be viewed in table
1.
Basicity test results in Table 1 showed that the rise of CaO mole in catalyst 5%
K2O / CaO-ZnO caused the basicity increase. Conversely, an increase of ZnO
mole in catalyst 5% K2O / CaO-ZnO caused the basicity go down. That is because
ZnO is a component in the catalyst support. ZnO is support of a catalyst which is
aims to increase the surface area, porosity, mechanical properties, and also
stability of the catalyst (Istadi, 2011). Thus, the increase of ZnO contribute to the
rise of surface area, not the increase of active site.
On the other hand, the rise of catalysts basicity because of a high number of
CaO, could be due to the value base of CaO is greater than ZnO. Strength bases
of alkaline earth metal oxides parallel by the size of alkaline earth metal atom
(Samik, 2015). The left side of Elements Periodic System, caused the alkaline
strength will increase. Atom of Ca is in group 2A, while Zn is in group 2B shows
that the power of alkaline Ca greater than Zn.

== This study, also carried out the preparation of catalyst K2O/(3: 1)CaO-ZnO
with variation of K2O percentage. The variation of K2O promoter given to CaOZnO catalyst aims to determine whether the addition of a promoter can increase

catalysts basicity. Addition of K2O promoter with different variations performed

on CaO-ZnO catalyst with mole ratio CaO: ZnO 3: 1. This research using catalyst
with mol ratio CaO:ZnO 3:1 as the basis catayst because in earlier test showed
that the catalyst 5%K2O/CaO-ZnO provides the highest value of basicity on mole
ratio of CaO: ZnO 3: 1. K2O promoter were added in CaO-ZnO catalyst with
variation range from 1%, 3% and 7%. Basicity test method using titration by benzoic acid and
benzene as the solvent, using bromotymol blue (BTB) show the result that can be viewed in figure 3.

Basicity test results in Figure 3 shows that the higher percentage of K2O in the
catalyst will increase its basicity. K2O promoter is a promoter which is designed
to assist active components and catalyst support (Istadi, 2011). Promoter aims to
generate activity, selectivity and stability of catalyst (Istadi, 2011). In CaO-ZnO
catalyst, K2O promoter supports the active catalyst component which is CaO
substance. Thus, an increase of K2O in the catalyst could support the presence
of CaO as catalytically active sites and cause catalysts basicity rise. Earlier, in
Table 1 shows a contrast between active component (CaO) and catalysts support
(ZnO). So that, the increase of basicity or active site of the catalyst may reduce
the function of catalysts support, such as surface area of catalyst.

== Biodiesel production is highly depend on the presence of a catalyst to

accelerate the transesterification reaction rate. Catalyst 5%K2O/CaO-ZnO has
been used for transesterification process to produce biodiesel from soybean oil.
This research set parameters such as, mole ratio of soybean oil and methanol
1:15, weight of catalyst 5% of weight soybean oil, time of transesterification 4
hours, reaction temperature 60 C, and constant stirring.
Biodiesel is the product result of transesterification process. The biodiesel then
tested its viscosity, density, acid number, and yield FAME. Viscosity test was
performed using Ostwald viscosimeter. Density test carried out using picnometer.
Acid number test was done by titration method using KOH solution as the titrane,
biodiesel as the titer, and phenolphtalein as the indicator. While, methyl esther
test within biodiesel was conducted by GCMS method. Biodiesel result based on
the catalysts used can be seen in Table 2.
Amount of methyl esters in biodiesel (FAME yield and yield biodiesel) is the most
important result in the process of transesterification. Yield FAME is influenced by
several factors such as %FAME, biodiesel volume and mass of the oil used during
the transesterification (oil mass constant at 227,7 gram). Whereas, yield of
biodiesel is not affected by %FAME. The value of yield FAME in biodiesel
indicates the presence of fatty acid methyl ester. Yield FAME and yield of
biodiesel results can be seen in Table 3.

==Determination of the best catalyst with mole ratio CaO: ZnO can be assessed
based on the value of the highest yield FAME (Puspitaningati et al, 2013). The
greater content of yield FAME, thehigher quality will be obtained. Biodiesel

quality requirements such as density, viscosity and acid number must agree with
the Indonesian National Standard (SNI). Where the SNI standard of biodiesel
include kinematic viscosity (2.3 to 6 mm2 / s), density (8500-890 kg / m3), and
the acid number (<0.5 mgKOH / g sample).
Based on the data obtained in Table 2 and Table 3, the mole ratio CaO:ZnO 1: 2
shows the highest yield FAME. Its viscosity, density, and acid number also meets
ISO standards. It concluded that the catalyst 5%K2O/CaO-ZnO with mole ratio of
1: 2 is the catalyst with the best results.

== Based on research that has been done can be concluded that:

1. Biodiesel could be produce through transesterification reaction of soybean oil
and methanol using alkaline solid catalyst 5%K2O/CaO-ZnO.
2. Characterization of catalyst 5%K2O/CaO-ZnO using XRD method showed the
presence of CaO, ZnO, and K2O in catalysts with different intensities, depending
on the mol ratio of CaO:ZnO.
3.Catalyst 5%K2O/CaO-ZnO with the highest basicity obtained at a mole ratio
CaO: ZnO 3: 1. Catalysts with the lowest basicity obtained at mole ratio CaO:
ZnO 1: 1. The higher moles of CaO in the catalyst will increase its basicity.
4. Addition of K2O promoter in CaO-ZnO catalyst can improve the basicity. The
higher number of K2O cause a higher basicity of catalyst. The highest basicity of
catalyst obtained by the addition of 7% K2O in the ratio mol CaO:ZnO 3: 1
5. Based on GCMS test, the catalyst which produces biodiesel with highest yield
FAME obtained at a mole ratio CaO:ZnO 1:2. The catalyst with mole ratio CaO:
ZnO 1:2 defined as the best catalyst because it produces the highest yield of
FAME.