Palm Oil-Based Lubricant Production using Pulsed Loop Reactor

Hamidah Abd Hamid

Sem. 1 (2011/2012)

12 January 2012

Topic description
Background
Statement of problem Objectives

Overall process flow

Research methodology Gantt chart Expected outcomes

Background
World demand for lubricants will rise more than 2% annually to 41 million

metric tons in 2015 (Freedonia Group Inc., 2011)

There are numerous applications of lubricants such as in automotive,

aviation, refrigeration and compressor, through the use of two stroke engine oils, automotive diesel oils, metalworking fluids, etc. oil-based lubricants:

Driving forces for the use of biodegradable lubricants instead of mineral Biodegradability - reduce environmental pollution Excellent lubricity Low volatility Renewability of the source Protection of workers health

Background
Polyol esters are excellent substitutes for mineral oils due to their high

thermal and oxidative stability, good lubricating properties and excellent viscosity-temperature properties (Randles, 2006)
Palm oil methyl esters (POME) are presently being promoted for

biolubricant production in Malaysia.

Polyol ester based on palm oil has been produced from the

transesterification of methyl esters with a well known polyhydric alcohol in lubrication field, which is trimethylolpropane (TMP) (Yunus et al., 2003; Beran, 2006).
Study shows that transesterification of POME with TMP has been

successfully produced in a conventional batch reactor (Yunus et al., 2004).

Background
The use of the sodium methoxide catalyst was to reduce the

side reactions that occur which often takes place when sodium hydroxide is employed as the catalyst.
The acid catalyst was also not preferable in the reaction due to

lower performance compared to the sodium methoxide catalyst in the esterification of vegetable lipids (Liu, 1994).
In our research, it is proposed to use calcium methoxide

instead of sodium methoxide due to its long lifetime that can maintain the catalyst activity and being reused for 20 cycles (Liu et al., 2008; Martyanov and Sayari, 2008).

Background
The transesterification of plant oil-based methyl ester with

trimethylolpropane is affected by various factors depending upon the reaction condition used. One of the most important parameters that affecting the reaction is the mixing efficiency (Meher et al., 2006).
liquid phases, the use of oscillatory flow mixing in pulsed loop reactor is proposed.

In order to improve mixing and mass/heat transfer between two

There were established studies in biodiesel production that proved

successful replacement of the classical mixing-heating conditions with the application of oscillatory flow mixing regarding the continuous transesterification of vegetable oils (Qiu et al., 2010; Zheng et al., 2007).

Background
Continuous pulsed loop reactor:

A potential alternative to replace batch reaction process.

A new type of tubular reactor containing equally spaced

baffles in vertical tubes operated and connected to each other by U-bend A pulsed (oscillatory) flow can be produced by using:

piston drive (fixed amplitude) or a pulsator (varied amplitude).

It enhances mass and heat transfer , intensifies radial mixing

and improves reaction time profiles (Harvey et al., 2003; Palma and Giudici, 2003).

Problem statement
Earlier studies focuses on the synthesis of palm oil-based polyol esters by

using a batch reactor. There were published studies on the application of pulsed flow mixing for the biodiesel production (Zheng et al., 2007; Qiu et al., 2010; Syam et al., 2011), but limited reports on pulsed flow reaction for biolubricant production. Lack of design information about pulsed flow reactor system for vacuum operating condition.
Thus, this study focuses on:
Design of a pulsed loop reactor for palm oil-based lubricant production

basis for scale-up purposes Filling the knowledge gap about pulsed flow reaction in vacuum condition.

Objectives

To design a pulsed loop reactor for the continuous production of palm oil-based trimethylolpropane (TMP) esters. To determine the optimum process conditions for the loop reactor. To study the kinetics of the reaction. To analyze the properties of palm oil-based TMP esters.

Overall process flow

POME Fractionation Unit Saturated POME TMP and calcium methoxide catalyst Gas Chromatography (GC) Analysis

Pulsed Loop Reactor

Separation Unit

Fatty soaps, catalyst

Purification Unit

Pure Biolubricant

GC analysis, product properties analysis

Overall research flowchart

Methodology Design the pulse loop reactor Response Surface Design (RSM) Synthesis of palm oilbased polyol esters Kinetic study and verification Analysis of Product Properties

Fabrication and commissioning the reactor

Optimization of process conditions

Experiments

RSM
Design Expert

Research methodology
1.

Reactor design (modification of the available biodiesel pulsed loop reactor)

Mass and Energy Balance determines the dimension of reactor

Mechanical design (corrossion allowance, baffle and tube design, heating jacket, pump specification)

verifies the feasibility of the proposed reactor dimension

Materials of Construction

determines the most economical material which satisfies both process and mechanical requirements to monitor the progress of reaction and to maintain the process at desired operating value

Control and Instrumentation

Research methodology
2.

Optimization
Controlled variable Oscillatory frequency ( 1 to 10 Hz) Molar ratio of POME to TMP (1-3: 1) Amount of catalyst (0.5 to 1 wt%) Pressure (0.5 mbar to 20 mbar) Reaction temperature (70 to 130 C) Residence time (1 min to 4 h) Response Product yield (palm oil-based polyol esters) Product yield Product yield Product yield Product yield Concentration of reaction mixture

3.

Kinetic Study
Controlled variable Temperature (70 to 130 C) Response Concentrations of reaction mixture

Research methodology
4.

Analysis of palm oil-based polyol esters (final product)

Important lubrication properties Kinematic viscosity (at 40 and 100 C) Viscosity index Pour point Frictional coefficient, Wear scar diameter (WSD) Acid number Unit ____(mm2/s) ____ ____( C) ____ ____ (mm) ____

Research Gantt chart

No. 1 2 3 4 5 6 7 8 Research Activities Literature search Problem identification and familiarization Reactor design Fabrication and commissioning of reactor Optimization of transesterification reaction Kinetic study on transesterification reaction Product analysis Preparation of thesis submission 1 2 3 4 5 6 Completion of Reactor Design Completion of Fabrication and Commissioning of Reactor Completion of Optimization of Transesterification Reaction Completion of Kinetics Study on Transesterification Reaction Product Analysis Final Thesis draft for submission (January 2012) (June 2012) (November 2012) (February 2013) (August2013) (January 2013) 2011 2012 2013 2014 O N D J F M A M J J A S O N D J F M A M J J A S O N D J F M

Research milestone

Expected outcomes
A n improved technology (rendering the downstream

separation processes easier) at lower residence time of transesterification between POME and TMP.

Thank You!