Effect of Moisture Content and Seed Rate of Calophyllum Inophyllum Oil

Extraction using Modular Screw Extruder

Yuli S. Indartono1,2, Heriawan1, I. Amalia Kartika3

1
Faculty of Mechanical and Aerospace Engineering, Institut Teknologi Bandung, Bandung,
40132, INDONESIA
2
Research Center on New & Renewable Energy, Institut Teknologi Bandung, 40132, Bandung,
INDONESIA
3
Department of Industrial Technology of Agriculture, Faculty of Agricultural Technology,
Institut Pertanian Bogor, Bogor, 16680, INDONESIA
Corresponding Author: Yuli S. Indartono, ysindartono@ditdik.itb.ac.id

Abstract-Oil extracted from Calophyllum inophyllum may be used as biofuel. This plant can be found on coastal
areas in Indonesia. This research investigates effect of moisture content and seed rate to the oil yield. Oil extraction
mechanism used in this study is modular screw extruder. The finding showed that oil extraction yield increased as
seeds rate is elevated. The optimum seed moisture-content is 5.53%, which produced oil yield of 50.25% (dry base).
The calophyllum oil was tested and compared to biofuel standard. Generally, the physicochemical characteristics of
calophyllum oil have met the biofuel standard, except its viscosity. Calophyllum oil can be used as biofuel by using a
preheater to reduce its viscosity.

Keywords: oil extraction, calophyllum, moisture content, seed rate

I. INTRODUCTION

Calophyllum tree produces a high fat and non-edible seeds. The fat content of these seeds in

dry state reaches 75%, which is higher than the Jatropha’s and the Rubber’s which are only around

of 40-60% and 40-50% respectively [1]. In Indonesia, this tree is the most widely grown vegetation

on the coastal area and can produce seeds between 40-150 kg/tree/year or around of 20 tons/ha/year

[2]. This production is higher than that of the Jatropha seeds (5 tons/ha/year) and the Palm seeds

(6 tons/ha/year) [2]. Oil yield of Calophyllum seeds of 12 populations in Indonesia varies between

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37-58% [2]. This yield is higher than Jatropha (25-40%), Adenanthera (14-28%), Sterculia (24-

40%), Schleichera (30-40%), and Moringa (39-40%) [2]. Therefore, Calophyllum seeds are

potential to be developed as biofuel, mainly to be used in remote or outer islands in Indonesia.

Because of that, Indonesian government plans to increase biofuel supplies for power generation

from 9% in 2014 to 30% in 2050 [3].

Since chemical availability in remote area maybe limited, mechanical extraction for

Calophyllum seeds is better than chemical extraction. Researches about mechanical calophyllum

oil extraction have been conducted by some researchers [1, 4, 5]. These studies reported three

different findings regarding the highest oil yield, namely 33.46% [1], 31.50% [4], and 45.50%

respectively [5] on dry seeds basis. Their test treatments focused on seeds moisture content and

seeds particle size.

Mechanical seeds extraction using flexible screw extruder had been conducted by some

investigators [6, 7, 8, 9]. Dufaure et al. [6] obtained the highest oil yield of Sunflower seeds at

120oC and natural moisture content of seeds at 5%. Amalia Kartika et al. [7] used the same

Sunflower seeds showed that the highest yield was obtained when operating conditions was at

120oC, 75 rpm, and seeds rate at 19 kg/h. Evon et al. [8] used Jatropha seeds showed that oil yield

systematically increased by reducing rotation speed and temperature.

Orhevba at al. [9] using screw press for neem seed kernel oil extraction found that the optimum

seed moisture content fall between 6.3 and 8.1%. From their study, they showed that there was

certain optimum seed moisture contents for the maximum oil yield for various seeds. Udoh et al.

[10] reported that moisture content had great influence on the amount of forces required to break

the seed.

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 The physicochemical characteristics of Calophyllum oil investigated by previous researchers

generally do not meet diesel oil standard. Fadhlullah et al. [1] produced Calophyllum oil with

viscosity of 56-108 cP. Amalia Kartika et al. [11] produced calopyllum oil with viscosity of 63-

65 cP and acid number of 34.83-54 mg NaOH/g. It is important to note that the Indonesian

government standard for biofuel requires maximum viscosity of 36 cP, maximum acid number of

2 g KOH/g, maximum iodine number of 115 g I2/100 g, and saponification number of 180-265 mg

KOH/g [12].

This study used single-shaft and modular-screw to extract oil from Calophyllum Inophyllum.

Best screw configuration and operating condition were investigated in previous study [13]. Effect

of seed moisture content and seed rate would be evaluated in this study.

II. RESEARCH METHODOLOGY

There were five steps in experiment: raw material preparation, seeds extraction, filtrate

filtration, oil purification, and oil physicochemical analysis. Variations of seeds moisture content

used in this study were 1.69%, 5.53%, 10.34%, and 12.80%. Seeds particle size was around of 5

mm. Requirement of seeds moisture content was established by the International Seeds Testing

Association (ISTA) [14].

Figure 1(a) shows some samples of Calophyllum seeds from Cilacap Regency, Central Java

Province, before it was dried. In the figure, seed-size is compared with 2.5 cm coin. Figure 1(b)

shows wrapped dried-Calophyllum seeds. Figure 1(c) shows Calophyllum seeds after pounded.

The drying process was carried out in the oven at a maximum temperature of 60°C until it reached

expected moisture content. After drying process, seeds were weighed per 500 g and wrapped with

3
aluminum foil to keep the water content unchanged. Two seeds samples were taken randomly to

be tested in a certified laboratory to check the actual percentage of water content.

FIG. 1 (a) Calophyllum seeds before being dried, (b) Calophyllum seeds after being dried and then wrapped with

aluminum foil to keep the water content unchanged, and (c) Calophyllum seeds after being pounded.

Modular-screw extruder can be seen in Figure 2. There were four types of screw: transport

screw (T), forward screw (F), reverse screw (R), and idle screw (I). These four types of screws had

different functions. Screw composition could be changed to get the best configuration. The

transport and forward screws provided pressure with a forward movement to the seeds particles.

Pressure provided by the transport screw was less than the pressure applied by the forward screw.

The reverse screw provided pressure with a backward movement to the seeds particles. The idle

screws only provided the pressure without giving a forward or backward movement to the seeds

particles. The forward screws had pitch lengths variations of 10 mm (F10), 16 mm (F16), 25 mm

(F25), 33 mm (F33), and 50 mm (F50) with uniform segment lengths of 10 cm. The reverse screws

had pitch lengths variations of 10 mm (R10), 16 mm (R16), and 25 mm (R25) with uniform

segment lengths of 5 cm. The transport screws had only 1 pitch length of 66 mm (T66) with

segment length of 10 cm. Meanwhile the idle screw is an oval-shaped screw, with diameters

variations of 34 mm (I34) and 38 mm (I38), with a segment length of 2 cm.

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 FIG. 2 Modular-screw extruder

The screws were arranged on a shaft. Length of screws configuration can be adjusted by

shifting barrel lock. In this study, length of shaft is 1 m. Two kinds of barrel filters were used in

this experiment: barrel 1 with 330 holes, and barrel 2 with 627 holes. Each hole has a diameter of

2 mm. The proper selection of screws arrangement, number of barrel filter holes, rotation speed,

and barrel temperature to produce high oil yield was investigated in previous study [13]. The oil

yield was calculated using Equation (1) i.e. the ratio between the mass of filtered oil (mo) and the

mass of the dried seeds (ms).

mo
𝑂𝑖𝑙 𝑦𝑖𝑒𝑙𝑑 (%) = x 100% (1)
ms

Vacuum filtration step was carried out to obtain Calophyllum oil free from impurities of seeds

particles. The vacuum filtration had a suction power of 5 Hp.

From the previous research [13], the best condition for oil extraction is: screw configuration

T66/F16/I34/I34/I34/I34/I34/F16/F10, barrel filter 2 (627 holes), rotation speed of 25 rpm, and

barrel temperature 60oC. This set-up is used for current study.

Oil purification step was done to improve the quality of Calophyllum oil by referring to the

procedures undertaken by Amalia Kartika et al. [11]. The procedure consisted of two main

processes, i.e. degumming to decrease the gum content and impurity compounds in oil, and

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neutralization to decrease the acidity of the oil. Oil purification was started by heating the oil up

to 70oC, adding 20% phosphoric acid solution by 0.2% (v/b), and stirring for 25 minutes while

maintaining the mixture at 70oC. NaOH solution with concentration of 18oBe was added into the

mixture, and stirred for 10-15 minutes. The process was continued by letting the mixture for

several days to produce sediment. After separating the oil from the solid sediment, the oil was

washed with water at 60-70oC to get neutral pH, and heated at 80oC to evaporate the water [11].

The last step was to analyze the physicochemical characteristics of Calophyllum oil, before

and after purification, and then it was compared to the standard characteristics of biofuel. This step

was done to determine the suitability of Calophyllum oil for diesel engine. The characteristics to

be analyzed were viscosity, acid number, saponification number, iodine number, and density.

III. RESULT AND DISCUSSION

A. Seeds moisture content

Based on the proximate test, it was known that Calophyllum seeds had high fat content, i.e.

around 53.29%. The water content reached 27.62%, and other contents such as ash, protein, and

carbohydrates around of 25.09%. In order to obtain oil as much as possible, the water content in

the seeds should be suppressed before mechanical extraction process.

Some researchers mentioned that the best moisture content of Calophyllum seeds that gave the

highest yield value was 1.2% [1] and 15% [5, 6]. Therefore, in this research, the seeds were treated

to get moisture content in range 1.2% until 15%. Seeds moisture content used in this study were

shown Table I.

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 TABLE I. Test results of water and fat content of Calophyllum seeds after dried

Actual Moisture Content Actual Fat Content

Target Moisture
(Dry Base) (Dry Base)
No Content (Dry
Deviation Deviation
Base) Average Average
Standard Standard
1 1.20% 1.69% 0.00% 71.20% 0.00%
2 5.00% 5.53% 0.29% 70.31% 0.16%
3 10.00% 10.34% 2.04% 65.46% 1.72%
4 15.00% 12.80% 0.06% 59.61% 5.56%

The difference between target and actual moisture contents is caused by the non-uniformity of

initial seeds moisture content. Therefore, when heating was done for a sample, the average of final

seeds moisture content was also not uniform. However, the average value of moisture content is

close to the target. Table I also informs that by decreasing moisture content cause increasing fat

content in the seeds.

Influence of seeds moisture content to the oil yield is given by Figure 3. The results showed

that the highest oil yield was obtained at 5.53% moisture content. Based on Table I, it can be seen

that the actual fat content (dry base) of seeds with moisture content of 1.69% and 5.53% were

close. However, higher water content in seeds with moisture content of 5.53% may facilitate seeds

breaking. After the optimum value, higher seeds moisture content gave lower oil yield. This trend

is actually typical for seeds oil extraction.

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 50.25

Oil Yield (%) 41.79

38.44
32.75

1.69 5.53 10.34 12.8

Moisture Content (%)

FIG. 3. Oil yield as function of seeds moisture content

B. Seeds rate

To evaluate the influence of seeds rate, best oil extractor set-up from previous study [13] was

used. Seeds moisture content used in this test was 5.53%. The result of seeds rate variation test is

given by Figure 4. Confirmed with expectation, oil yield was higher when seeds rate was higher.

This result is the same with the research of Dufaure et al. [6] and Amalia Kartika et al. [7]. Then,

it can be stated that higher seeds rate is responsible for higher seed density and it increases axial

force. As a result, the pressure received by the material increases and then triggers higher oil yield.

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 36.09

Oil Yield (%)

33.42
32.75

1.5 3 5
Seeds Rate (kg/h)

FIG. 4. Oil yield result from seeds rate variation tests

Oil filtration technique used in this study was vacuum filtration. The filtrate by centrifuge

filtration was wetter than vacuum filtration as shown in Figure 5. This indicates that the filtrate

residue still contained a lot of oil. While residues from vacuum filtration shows dryer condition.

FIG. 5 (a) Residues were produced by centrifuge filtration and (b) Residues were produced by vacuum filtration.

Oil extraction with seeds moisture content of 5.53% and seeds rate of 5 kg/h produced

extraction efficiency of 71.47%. Extraction efficiency is a ratio between oil produced and total oil

content in the seeds after they were dried.

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C. Purification and physicochemical analysis

Purification process was done by degumming and neutralization. The results of purification and

chemical analysis of Calophyllum oil are given by Table II. Based on the table, purification process

of Calophyllum oil causes mass loss up to 47.15%.

TABLE II. Physicochemical characteristics analysis of Calophyllum oil before and after purification.
Result
Parameter Unit Before After Method
Purification Purification
Mass g 40.460 21.383 Kartika et al. [11]
Density g/mL 0.905 0.879 ASTM D 1298
Kinematic viscosity mm2/s 103.23 60.828 ASTM D 445
Acid number mg KOH/g 54.179 0.999 AOCS Cd 3-63
oil
Saponification mg KOH/g 207.448 203.737 AOCS Ca 14-56
number oil
Iod number g I2/100 g oil 93.028 86.696 AOCS Cd 1-25

Comparing properties in Table II with the Indonesian government standard for biofuel [11], most

of the oil properties are suitable to be used as fuel, except the viscosity. The standard [11] requires

that biofuel should have a density of 0.90-0.92 g/mL, maximum viscosity of 36 mm2/s, maximum

acid number of 2 mg KOH/g, saponification number of 180-265 mg KOH/g, and maximum iod

number of 115 g I2/100 g. To reduce the viscosity of Calophyllum oil, a preheater should be applied

before the oil enter combustion chamber.

IV. CONCLUSIONS

This study evaluated the best condition to extract Calophyllum Inohyllum oil by using

modular-screw extractor. Focus of this research was the influence of seeds moisture content and

10
seeds rate to the oil extraction yield. Psycochemical properties of Calophyllum Inophyllum oil

were checked and compared to the biofuel standard. This study concluded that the best moisture

content was 5.53% (dry base). This study confirmed that higher seeds rate produces higher oil

yield. Oil yield (50.25%) and extraction efficiency (71.47%) resulted from this experiment was

higher than similar work done by other researchers [1,4,5].

Purification process by degumming and neutralization improved acid number, saponification

number, density, and iodine number, and viscosity. However, the viscosity after purified was still

higher than the standard fuel viscosity. A preheater may be used to reduce the viscosity before the

oil entered the combustion chamber.

ACKNOWLEDGMENTS

This work was funded by Outstanding and Strategic National Research/Penelitian Unggulan

dan Strategis Nasional (PUSNAS) project 2015-2017 and Research, Community Service, and

Innovation Program/Program Penelitian, Pengabdian kepada Masyarakat, dan Inovasi (P3MI)

project 2017.

REFERENCES

1
Fadhlullah M., Sri Nanan B. Widiyanto, and Elvi Restiawaty, “The potential of nyamplung (Calophyllum

inophyllum L.) seeds oil as biodiesel feedstock: effect of seeds moisture content and particle size on oil yield”, 2nd

International Conference on Sustainable Energy Engineering and Application, ICSEEA, pp. 177-185, 2015.
2
Leksono Budi, Sekilas tentang Nyamplung (Calophyllum inophyllum L.), Balai Besar Penelitian Boteknologi

dan Pemuliaan Tanaman Hutan Yogyakarta, 2012.

3
Badan Pengkajian dan Penerapan Teknologi Report, OUTLOOK ENERGI INDONESIA 2016, Badan

Pengkajian dan Penerapan Teknologi, 2016.

11
 4
Jahirul M. I., Brown J.R., Senadeera W., Ashwath N., Laing C., and Leski Taylor J, “Optimisation of Bio-Oil

Extraction Process from Beauty Leaf (Calophyllum inophyllum)”, 5th BSME International Conference on Thermal

Engineering, Procedia Engineering 56, pp. 619-624, 2013.

5
Bhuiya M. Rasul M. K., M. G., Khan M. M. K., Ashwath N., Azad A. K., and Mofijur M, “Optimisation of

Oil Extraction Process from Australian Native Beauty Leaf Seeds (Calophyllum inophyllum)”, 7th International

Conference on Applied Energy-ICAE 2015, Energy Procedia 75, pp. 56-61, 2015.
6
Dufaure Corinne, Juliette Leyris, Luc Rigal, and Zephirin Mouloungui, “A twin-screw extruder for oil

extraction: I. direct expression of oleic sunflower seeds”, JAOCS, U.A. INRA 31A1010, Vol. 76, No. 9, 1999.
7
Amalia Kartika I., Pontalier P.Y., and Rigal L, “Extraction of sunflower oil by twin screw extruder: screw

cconfiguration and operating condition effects”, Bioresource Technology 97, pp. 2302-2310, 2006.
8
Evon, Ph., I. Amalia Kartika, M. Cerny, and Rigal L, “Extraction of Oil from jatropha seeds using a twin-

screw extruder: feasibility research”, Industrial Crops and Products 47, pp. 33-42, 2013.
9
Orhevba B. A., O. Chukwu, Z. D. Osunde, and V. Ogwuagwu, “Influence of Moisture Content on The Yield

of Mechanically Expressed Neem Seed Kernel Oil”, Natural and Applied Sciences Vol. 4 No. 5, pp. 252-257, 2013.
10
Udoh Juliet E., Tajudeen M. A. Ulayanju, Olawale U. Dairo, and Akindele F. Alonge, “Effect of Moisture

Content on the Mechanical and Oil Properties of Soursop Seeds”, Chemical Engineering Transactions, 58, DOI:

10.3303/CET1758061, pp. 361-366, 2017

11
Amalia Kartika I, Syelly Fathiyah, Desrial, and Yohanes Aris Purwanto, “Pemurnian Minyak Nyamplung

dan Aplikasinya sebagai Bahan Bakar Nabati”, J. Tek. Ind. Pert. Vol. 20(2), pp. 122-129, 2012.
12
Direktorat Jenderal Energi Baru, Terbarukan, dan Konversi Energi Report, Standar dan Mutu (Spesifikasi)

Bahan Bakar Nabati (Biofuel) Jenis Minyak Nabati Murni untuk Bahan Bakar Motor Diesel Putaran Sedang.

Direktorat Jenderal Energi Baru, Terbarukan, dan Konversi Energi, 2013.

13
Heriawan, Yuli S. Indartono, and Ika Amalia Kartika, “Optimization of Mechanical Oil Extraction Process

of Nyamplung Seeds (Calophyllum inophyllum L.) by Flexible Single Screw Extruder”, The International Conference

of Thermal Science and Technology, Bali, 2017

14
International Seeds Testing Association Report, International Rules for Seeds Testing, International Seeds

Testing Association, 2015.

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