 *Corresponding author.

Email: mursalin@unja.ac.id

eISSN: 2550-2166 / © 2020 The Authors. Published by Rynnye Lyan Resources

  Food Research 4 (4) : 1011 - 1017 (August 2020)
  Journal homepage: http://www.myfoodresearch.com

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Purification engineering of mono-diacylglycerol using creaming demulsification

technique in 20 kg-scale

*Mursalin, M., Sahrial, S. and Yernisa, Y.

 Faculty of Agricultural Technology, Universitas Jambi, Jalan Raya Jambi-Muara Bulian Km.15 Mendalo

Darat, Jambi 36122, Indonesia

Article history:

Received: 29 October 2019

Received in revised form: 12

February 2020

Accepted:  14 February 2020

Available Online: 12 March

2020

Keywords:

Demulsification,

Glycerolysis,

Nozzle,

Mono-diacylglycerol,

Purification

DOI:
https://doi.org/10.26656/fr.2017.4(4).360

Abstract

Glycerolysis is the easiest, cheapest, and most widely used method for producing mono-

diacylglycerol (MDAG). The crude MDAG resulting from chemical glycerolysis still

contains a glycerol residue of more than 7.5% so it needs to be purified. Purification with

a simple method using a creaming demulsification technique (CDT) on a laboratory scale

has been proven to produce MDAG with a glycerol content of less than 1%. This study

was aimed to apply CDT on a scale of 20 kg and determine the process conditions that

need to be adjusted so that the results are not different from the laboratory scale. Through

trial and error method, the process condition adjustment was done iteratively to produce

MDAG glycerol content after purification of less than 1.5%. The initial content of crude

MDAG was 12.48%, application of CDT on a scale of 20 kg produces pure MDAG with a

glycerol residue content of 3.07% (without adjusting the process conditions) and was

1.15% (with adjusting the process conditions).  The adjustments meant include: increasing

the operating temperature from 65 to 70°C, changing the type of stirrer from a propeller

into a 2-level impeller, applying the nozzle for electrolyte mixing, providing longer skim

and cream separation opportunities (applying repeated settling), using 1.5 times more hot

water for washing, the washing technique was set twice, the first washing using nozzle

without stirring and the second using nozzle with stirring.  The adjustments were able to

increase the purity of the MDAG produced and has met the European Union and FAO/

WHO standards.

1. Introduction

Glycerolysis is the easiest, cheapest, and most

widely used method for producing mono-diacylglycerol

(MDAG) (Cheng et al., 2005; Chetpattananondh and

Tongurai, 2008; Galucio et al., 2011). MDAG produced

from the glycerolysis still contains quite high glycerol

residues, between 16.61–19.04% (Rachmawati, 2017)

and 7.26–12.29% (Agustina, 2019). The presence of

glycerol in MDAG reduces MAG levels, causes off

color, decreases the melting point (Laksana, 2016), and

reduces the ability of the product as an emulsifier

(Moonen and Bas, 2015). According to European Union

regulations (EEC-E471), the maximum limit of glycerol

content in MDAG is 7% (Hasenhuettl, 2008). Therefore,

purification is needed to separate the glycerol residue

from the crude MDAG. MDAG purification could be

carried out by Short Path Distillation (SPD) (Rossi et al.,

2012; Zhang et al., 2014), solvent extraction

(Rumondang et al., 2016; Sanchez et al., 2018), solvent

extraction and molecular distillation (Mardaweni et al. ,

2017), solvent saponification and extraction

(Setyaningsih et al., 2016) and creaming demulsification

technique (CDT) (Mursalin, Lavlinesia and Yernisa,

2017; Mursalin, Sahrial and Wulandari, 2017).

Purifying MDAG using molecular distillation

requires a large cost and special expertise to operate it,

this method is difficult to apply widely (Sanchez et al.,

2018). Purification by solvent extraction also has

disadvantages because of the possibility of the remaining

solvent in the final product. In addition, time-consuming

and decreasing yield are other disadvantages of this

method (Sanchez et al., 2018). Thus, CDT becomes a

new method of purifying MDAG which is more efficient

than molecular distillation and solvent extraction,

especially in separating glycerol residues.

The principle of CDT in purifying MDAG is by

destroying the stability of the emulsion system where

glycerol is dispersed. Demulsification occurs due to the

change in the emulsion system w/o to o/w (due to the

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addition of aqueous electrolyte solution), heating,

stirring, and separation of creams and skim (Mursalin,

Lavlinesia and Yernisa (2017). Three types of electrolyte

solutions that have been analyzed for their effects in

removing glycerol from MDAG produced by

glycerolysis are NaCl, CaCl2, and Ca(NO3)2.4 H2O.

MDAG purification process with 5% NaCl solution can

reduce glycerol from 14.99% to 1.64%, while with 5%

CaCl2 solution can reduce glycerol from 14.99% to

0.70% (Mursalin, Lavlinesia and Yernisa (2017). The

5% Ca(N03)2.4H2O solution can reduce glycerol levels

from 11.69±0.88% to 0.57±0.07% (Putri et al., 2019).

The optimum operating temperature is 60-70oC, stirring

at 400 rpm, and separation of the skim by sinking and by

centrifugation (Mursalin, Lavlinesia and Yernisa (2017).

MDAG purification with CDT on a laboratory scale

developed by Mursalin, Lavlinesia and Yernisa (2017)

was carried out with typical processing steps. The crude

MDAG was preheated in a beaker until the temperature

of 65oC was reached and all the crystals melt. 500 mL of

liquid MDAG (M1) at 65oC was put into the reactor, then

500 mL of electrolyte solution with a concentration of

5% (w/v) at 10oC above the temperature M1was also

inserted into the reactor and stirring at 500 rpm for 40

mins. After that, the mixture was deposited for 10 mins

(separation I) and then the skim fraction was separated

and cream 1 (M2) were collected. Then, M2 was then

washed by adding 1:1 (v/v) hot water at a temperature of

10oC above the temperature of M2. During the washing

process, the mixture was stirred 500 rpm for 10 mins at

65oC. After that, the mixture was re-deposited for 10

mins (separation II). This deposition will produce 3

layers in the form of cream II, intermediate, and skim II.

Then, cream II was centrifuged 2000 rpm for 5 mins, to

produce pure MDAG (M3) with glycerol residue content

of less than 1%.

For a scale of 20 kg, it is estimated that process

engineering is needed in order to allow the purification

method applied productively. The engineering includes

operational temperature, type of stirrer, mixing method,

amount of hot water, washing method, and sedimentation

time. The purpose of this research was to apply CDT on

a scale of 20 kg and determine the process conditions

that need to be adjusted so that the results are not

different from the laboratory scale.

2. Materials and methods

The main material used was MDAG from Fully

Hydrogenated Palm Kernel Oil (FHPKO) produced by

chemical glycerolysis, obtained from the SEAFAST

Center of IPB (Bogor, Indonesia). Other materials are

Distillated Monoglyceride from Rikevita Malaysia Sdn.

Bhd. (Johor, Malaysia), rac-1-Lauroylglycerol from

Sigma Aldrich (Germany), N-methyl-N-(trimethyl silyl)-

trifluoro acetamide from Sigma Aldrich (St. Louis, MO),

calcium nitrate tetrahydrate from PT. Setia Guna (Bogor,

Indonesia), tetrahydrofuran (Merck), and heptane

(Merck).

Process equipment used includes a set of reactors

with a capacity of 20 L made of stainless steel which is

equipped with agitators, heaters, tanks for electrolyte

solutions, water pumps, and nozzle systems. Av20 kg

scale purification reactors used in this study mimicked

the purification reactors used on a laboratory scale.

Analysis of the composition of the acylglycerol

fraction was using the Official Method Cd 11b-91

modification method (AOAC, 2003). Crude MDAG and

pure MDAG were each analyzed using Gas

Chromatography (GC) FID (Hewlett Packard series 6890

series DB5 HT column). The yield of pure MDAG was

determined by comparing the volume of pure MDAG

with the volume of crude MDAG multiplied by 100%.

The engineering implementation of the MDAG

purification process was carried out with trial and error

which refer to the technique was developed by Mursalin,

Lavlinesia and Yernisa (2017) in laboratory scale. The

data obtained was an average of three replications ±

standard deviations.

3. Results and discussion

3.1 Application of CDT on a scale of 20 kg without

"scaling-up adjustment"

CDT is an MDAG purification method with a

working principle based on the destruction of the

emulsion system through the formation of creams and

skims due to the application of temperature, stirring, and

the addition of an appropriate electrolyte solution. At the

laboratory scale, MDAG purification was carried out by

mixing liquid MDAG and electrolyte solution with the

same amount, at a temperature of electrolyte solution

10oC higher than MDAG’s. During the purification

process, the temperature and stirring were kept constant

at 65oC and 400 rpm, respectively. The function of

stirring is to facilitate the occurrence of oil droplets

collision easily and intensely allows floc being formed

quickly Mursalin, Lavlinesia and Yernisa (2017).

Crude MDAG containing glycerol as shown in Table

1, was quite high, which was 12.69%; after purification

with a method similar to that done on a laboratory scale

CDT, the glycerol content dropped to 3.07%. This shows

that the application of CDT on a scale of 20 kg even

without the scaling up adjustment, has been quite

successful in reducing the glycerol content of MDAG.

However, we are not yet satisfied with the pure MDAG

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results, where the glycerol residual content was still

more than 1.5%. Therefore engineering efforts in the

form of adjusting the process conditions were carried

out. MDAG chromatograms before and after purification

were illustrated in Figure 1.

The MDAG glycerol content before purification on

the chromatogram appeared at the 3.302 mins which was

12.69% (Figure 1A) and after purification, it appeared at

the 2,451 and 3,225 mins which were 3.07% (Figure

1B). The 20 kg scale MDAG Purifier was illustrated in

Figure 2 and the pure MDAG product in Figure 3.

3.2 Application of CDT on a scale of 20 kg with "scaling

-up adjustment"

The experimental results of using a 20 kg scale

MDAG purification reactor with adjustments to several

indicators of the engineering process were proven to

reduce the glycerol content in the final product to only

1.15%. The intended engineering included increasing the

operating temperature from 65 to 70°C, changing the

type of stirrer from a propeller into a 2-level impeller,

applying the nozzle for electrolyte mixing, providing

longer skim and cream separation opportunities

(applying repeated settling), using 1.5 times more hot

water for washing, the washing technique was set twice,

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Parameters
MDAG’s Characteristics

Before Purification After Purification

Faction Composition
•         MAG (%) 29.93±1.89 33.76±1.19

•         DAG (%) 28.63±2.87 31.61±1.05

•         TAG (%) 27.72±2.74 29.78±1.07

Total Glycerol (%) 12.48±0.29 3.07±0.05

Acid Numbers (mg KOH/g) 6.56±0.31  6.67±0.27

Free Fatty Acids (%) 2.34±0.11 2.86±0.14

Water (%) 1.06±0.14 2.06±0.17

Iod Number (g / 100 g) 0.31±0.00 0.31±0.00

Slip Melting Point (oC) 39-41 40-42

Color Brownish white Brownish white

Table 1. Comparison of MDAG before and after purification

Figure 1. MDAG chromatogram before purification (A) and after purification (B) using the CDT method on a scale of 20 kg

(A)

(B)

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the first washing using nozzle without stirring and the

second using nozzle with stirring.

The stages of applying CDT to purify MDAG on a

scale of 20 kg become slightly different from the

laboratory scale. The first stage, 20 kg of crude MDAG

was put into the reactor tank and heated while stirring at

400 rpm until a temperature of 70oC (not 65oC) is

reached. Meanwhile, 20 L of 5% calcium nitrate

tetrahydrate electrolyte solution was also heated in

another tank to a temperature of 80oC. Second stage,

after the MDAG temperature had been reached 70oC, the

heater was turned off but stirring continues. Five mins

later, the 80oC electrolyte solution was pumped and

sprayed through eight nozzles found at the top of the

tank. The pressure of the electrolyte solution produced

from the nozzle was estimated to be quite strong and

evenly distributed (hence there was no need to stir), as a

result polar components dispersed as impurities

(including glycerol) in MDAG would be carried to the

bottom of the tank and separated as a skim. During this

process, the temperature was maintained at 70oC, stirring

was stop, and the settling was applied. This settling lasts

for 15 mins or until the skim was separated from the

cream phase (M1). In the third stage, the stirrer was

turned on again at 200 rpm for 5 mins. Settling for 15

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Figure 2. MDAG Purifier scale of 20 kg

Figure 3. MDAG products purified from the 20 kg scale CDT

method

Figure 4. MDAG chromatogram before purification and consistency 3 times the purification result by adjusting the process

indicator, red circles indicate changes in the content of glycerol residues in the product

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mins after the process had obtained cream phase (M2)

and the second skim phase. Meanwhile, as much as 30 L

of distilled water was heated to a temperature of 80oC.

At the fourth stage, 15 L of 80°C distilled water was

sprayed through the nozzle into the reactor containing

M2, and allowed to mix without stirring. The temperature

of the mixture was held constant at 70oC and the mixture

of MDAG with aquadest was allowed to separate into

cream (M3) and skim phase, again. In the fifth stage,

after all the skim had been removed, 15 L of distilled

water at 80°C was re-sprayed through the nozzle into the

reactor containing M3 and allowed to mix without

stirring and it took about 15 mins until the fourth cream

and skim were separated. Finally, after all the skim from

the forth phase had been removed, the cream from the

forth phase (pure MDAG) was obtained.

The 20 kg scale MDAG refining technique

succeeded in reducing the glycerol levels in MDAG from

an initial concentration of 12.49±0.29% to 1.15±0.03%

(Table 2). This showed that by adjusting several process

conditions (temperature, type of stirrer, applying the

nozzle, repeated settling, and increasing of hot water for

washing), refining MDAG on a scale of 20 kg could be

as effective as on a laboratory scale. MDAG

chromatograms, before and after purification was

illustrated in Figure 4.

The results of GC analysis (Figure 5), showed that

MDAG before purification contained MAG, DAG, and

TAG of 29.93±1.89%, 28.63±2.87%, and 27.72±2.74%,

respectively. The raw material acylglicerol fraction in

this study was different from that reported by Mursalin,

Sahrial and Wulandari (2017) which was 32.27%

(MAG), 11.84% (DAG), and 33.62% (TAG). This

difference according to Triana (2014), occurred because

during the process of chemical glycerolysis not all fatty

acids could be released and react with glycerol.

Purification without adjustment produces MDAG

with MAG, DAG, and TAG contents of 33.76±1.19%,

31.61±1.05%, and 29.78±1.07%, respectively. MDAG

from the purification results with adjustments containing

MAG, DAG, and TAG were respectively 33.53±1.15%,

32.97±0.90%, and 32.35±1.11% (Table 2). Mursalin,

Sahrial and Wulandari (2017) reported that MDAG from

Fully Hydrogenated Palm Kernel Oil (FHPKO) purified

by CDT containing MAG, DAG, and TAG were 36.24%,

17.42%, and 37.67%, respectively. The percentage of

MAG and TAG in this study was lower than the results

of Mursalin, Sahrial and Wulandari (2017), but the

percentage of DAG was much higher. It was due to

differences in the composition of the acylglicerol

fraction of the crude MDAG used.

Based on Figure 5, the MAG and DAG content of

the product increased from the initial content in the raw

material. Similar to what was reported by Mursalin,

Sahrial and Wulandari (2017), MDAG purification

increased the MAG, DAG, and TAG content due to

decreased glycerol content. The percentage of pure

MDAG yield resulting from purification without and

with adjustments was 80.00±4.00% and 81.00±3.61%,

respectively. These results are not much different from

those produced by Moura et al. (2011a) and Moura et al.

(2011b), who conducted research on refining MDAG

from the same raw material, namely FHPKO, which was

76-95%.

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Parameters
MDAG’sCharacteristics

Before Purification Purification without Adjustment Purification with Adjustment

Faction Composition
•       MAG (%) 29.93±1.89 33.76±1.19 33.53±1.15

•       DAG (%) 28.63±2.87 31.61±1.05 32.97±0.90

•       TAG (%) 27.72±2.74 29.78±1.07 32.35±1.11

Total Glycerol (%) 12.48±0.29 3.07±0.05 1.15±0.03

Acid Numbers (mg KOH/g) 6.56±0.31  6.67±0.27  5.63±0.21

Free Fatty Acids (%) 2.34±0.11 2.86±0.14 2.78±0.13

Water (%) 1.06±0.14 2.06±0.17 3.19±0.16

Iod Number (g / 100 g) 0.31±0.00 0.31±0.00 0.31±0.00

Slip Melting Point (oC) 39-41 40-42 40-41

Color Brownish white Brownish white Brownish white

Table 2. Characteristics of MDAG before and after purification

Figure 5. Changes in the MDAG acylglicerol fraction before

purification, purification 1 (without adjustment of process

parameters), and purification 2 (by adjusting process

parameters)

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4. Conclusion

MDAG purification at a scale of 20 kg will be as

effective as a laboratory-scale if done by adjusting the

following process conditions: increase the operating

temperature from 65 to 70oC, changing the type of stirrer

from a propeller into a 2-level impeller, applying the

nozzle for electrolyte mixing, providing longer skim and

cream separation opportunities (applying repeated

settling), using 1.5 times more hot water for washing,

and the washing technique was set twice.  By this

technique, the pure MDAG could be produced

containing 1.15% glycerol residue, meet the European

Union and FAO/WHO standards.

Conflict of Interest

The authors declare that there are no conflicts of

interest.

Acknowledgments

The author would like to thank the Director of

Research and Community Service (DRPM) Ministry of

Research, Technology and the Higher Education

Republic of Indonesia for providing funds for the

implementation of this research.

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