By

NIK NORULAINI NIK AB RAHMANUNIVERSITI SAINS MALAYSIA

PENANG

3RD International conference on Advances in Engineering and Technology,

Dynasty Hotel , 26 and 27th Dec 2014, Kuala Lumpur, Malaysia

Basic science concepts in extraction

What is Supercritical fluid?

Supercritical fluid : An extraction technology

Supercritical fluid CO2 (SC-CO2) as solvent

Advanced engineering : SC-CO2extraction of oil system

Solute

Solvent

Polar and non polar

Solubility

Density

Pressure

Temperature

Diffusivity

Typical solvents for extraction are in liquid form.

What about gas as a solvent?What if gas is compressed ?Technology available to compress

gas...to a critical point.

Technology is available to compress gas to a supercritical level (beyond its critical point) converting gas to fluid, called supercritical fluid (SCF).

TTc = 31.1 oC

Pc

= 7

.38 M

Pa

solid

gas

liquid

Supercritical fluid

regionCritical point

P

The phenomenon of supercritical fluids (SCFs) was first discovered by a Frenchman Baron Charles Cagniard de la Tour in the early 1800s.

The dissolution of solutes in a supercritical fluid (SCF) medium was first observed by Hannay and Hogarth (1879)

Although SCFs were discovered in 1800s, as a technique, they were not utilized until the 1970s.

In 1970, SCFs were used commercially to

decaffeinate coffee - supercritical fluid extraction (SFE) as a technology

SFE technology is becoming an important processing procedure and is employed in a wide range of applications.

Proven to be an alternative refining process in extracting enriched solutes such as wheat germ oil (Eisenmenger and Dunford, 2008), rice bran oil (Kim et al., 1999, Chen et al., 2008), and crude PO and its components (Birtigh et al., 1995 ; Davarnejad, et al., 2008).

SFE technology has been used successfully to extract analytes from a variety of complex compounds through a manipulation of the system pressure and temperature (Fahlman, 2002).

SFE technology has been demonstrated to be a technique that eliminates some of the tedious steps of liquid–liquid and solid–liquid extraction procedures (McNally et al., 1992).

The SCF properties and characteristics, as a solvent

The application of the SCF solvent in the extraction,

The extraction influencing factors

The solute solubility in the SCF

The density of supercritical fluids is 100 to 1000 times greater than that of its gas and approaching to that of its liquid.

The adjustment of the density by changing the pressure and temperature

This makes the solvating power of supercritical fluid near to that of its liquid.

What gas do we choose?

Common solvent CO2 - converted from gas to fluid

Supercritical fluid CO2 or SC-CO2

IN THE EXTRACTION OF OIL

Noncombustible nor explosive, is environmentally friendly

CO2 good solvent for many organic compounds. SC-CO2 has relatively low viscosity and high diffusivity

(the diffusivity of SC-CO2 is 10−4 cm2 s−1 while that of liquid solvents is 10−5 cm2 s−1).

Enable the separation of compounds to be extracted due to its low viscosity, high diffusivity and the ability to solvate.

In SC-CO2 extraction, the fluid is continuously forced to flow through the samples; therefore, it can providequantitative or complete extraction.

These properties make SC-CO2 a good solvent for extraction.

Properties and Characteristics of

Supercritical CO2 as Extraction Solvent

0

5

10

15

20

25

30

0 200 400 600 800 1000 1200

density [kg/m 3]

P [M

Pa]

40

20 oC

5060

70

80 oC

A density based model proposed by Chrastil(Chrastil, 1982) - relates the solubility of solute (oil) to the density of solvent (SC-CO2) at a particular temperature.

Méndez-Santiago and Teja model - used to correlate solubility data of solutes in SC-CO2 to density (Méndez-Santiago and Teja, 1999, Méndez-Santiago and Teja, 2000).

0.00

0.01

0.02

0.03

0.04

0.05

310 320 330 340 350 360

So

lub

ilit

y [

g/g

]

Temperature [K]

20.7 MPa 24.1 MPa 27.6 MPa 31.0 MPa 34.5 MPa

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

0 50 100 150 200

Ext

ract

ed o

il [

g]

Carbon dioxide used [g]

CER slope of curve 1 ( ) : 0.0415

CER slope of curve 2 ( ) : 0.0417

CER slope of curve 3 ( ) : 0.0392

Average CER slope of the curves: 0.0408

1

3

2

In early extraction, the extraction curve shows a linear correlation between CO2 used and mass of the extracted oil [ CER ]

ADVANCED ENGINEERING :

SC-CO2 EXTRACTION

SYSTEM

Improving the technology, engineers consider

Design Factors that can influence the outcome of the extracted products e.g. the bed geometry, number of extraction and separation vessels, and solvent flow rate (Reverchon and Marrone, 2001).

knowledge of the phase equilibrium for the system as well as the solubility, diffusivity, and mass transfer rate for the overall process

1/22/2015SC-CO2 REFINED AND BLEACHED

PALM KERNEL OIL 24

THE ENGINEERING DRAWING FOR THE BUILDING OF A SCCO2 PILOT PLANT FOR OIL EXTRACTION

INITIATION OF THE CONSTRUCTION OF THE SCCO2 PILO T PLANT

MALAYSIAN RESEARCHERS AND JAPANESE MAKERS MAKE A TEAMWORKING ON THE CONSTRUTION OF THE SC-CO2 PILOT PLANT

A CHEMICAL ENGINEER CHECKING THE SYSTEM AGAINST THE ENGINEERING DRAWING

THE ENGINEER CHECKING THE EXTRACTED OIL

1/22/2015 29

d

A: The pilot plant of supercritical fluid extraction for palm kernels

B: Loading of palm kernels

C: Palm kernel oil collected

D: Palm kernel fiber

SYSTEM TESTED AND COMPLETED

1/22/2015SC-CO2 REFINED AND BLEACHED

PALM KERNEL OIL 31

1/22/2015

SC-CO2 REFINED AND BLEACHED PALM KERNEL OIL 32

Initial file date :MY128728(A)Title: Process for a Simultaneous Extraction and Fractionation of Palm Kernel Oil UsingSupercritical Carbon Dioxide as a SolventApp. Date: 28-February-2007Applicant: UniversitiSains Malaysia

1/22/2015SC-CO2 REFINED AND BLEACHED

PALM KERNEL OIL 33

Liq

uid

CO

2

Steriliza

tion

Vesse

l

Chiller

0~ 100C

2000 kcal/h

Cooler CO2

PumpPreheater

DP: 10

MPa

DT: 400C

230 kcal/h

DP: 60 MPa

Q: 10~

150mL/min

DP: 60

MPa

DT: 800C

3kW, ALC

Band

Heater

1kW

Open/Close

V01

V02 V03

Mathematical modeling of Enterococcus faecalis, Escherichia coli, and Bacillus sphaericus inactivation in infectious clinical solid waste by using steam autoclaving and supercritical fluid carbon dioxide sterilization. Md Sohrab Hossain, Nik Norulaini Nik AbRahman, Venugopal Balakrishnan, Mohd Omar Ab Kadir

Chemical Engineering Journal (Impact Factor: 3.47). 07/2014; DOI: 10.1016/j.cej.2014.07.097

ABSTRACT In the present study, steam autoclaving and supercritical carbon dioxide (SC-CO2) were utilized to inactivate Enterococcus faecalis, Escherichia coli, and Bacillus sphaericus in clinical solidwaste. The success of steam-based bacterial sterilization depends on temperature, treatment time, and the bacterial species present. Autoclave sterilization was found to be most effective at 121°C for 60 min and 131°C for 30 min. Complete inactivation of bacteria in clinical solid waste subjected to SC-CO2 sterilization was obtained after 30-120 min at a treatment range of 10-40 MPa and 35-80°C. The bacterial inactivation curves, which were generated using a modified Gompertzmodel to describe the relationship between survival rate and treatment time,was divided into three distinct phases.

It is imperative for us to understand the relationship between science and technology, and engineering.

Knowledge in Science precedes technology; and engineering uses technology - connected and influenced one another.

Super critical fluid extraction is a technology that synergize the knowledge of science into technology and engineering

Thank you