SPE-193449-MS

Investigating the Potential Use of Waste Vegetable Oils to Produce Synthetic

Base Fluids for Drilling Mud Formulation

O. K. Dankwa, S. S. Ackumey, and R. Amorin, University of Mines and Technology

Copyright 2018, Society of Petroleum Engineers

This paper was prepared for presentation at the Nigeria Annual International Conference and Exhibition held in Lagos, Nigeria, 6–8 August 2018.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
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Abstract
The environmental challenges posed by conventional oil-based drilling fluids along with legislation
associated with their use have necessitated the development of synthetic organic liquids that are designed
to improve environmental protection. In this research, waste/used oils from restaurants and food joints have
been tested for their potential use as synthetic based fluids through rheological analysis. Physiochemical
properties of the waste vegetable oil were determined; density: 0.88g/cm3, acid value: 64.8mg KOH/g of oil
and Free Fatty Acid (FFA) content: 32.4%. The optimum conditioning of biodiesel production from waste
oil was in two-step catalysed process. In the first step, sulfuric acid was used as a catalyst for esterification
reaction to reduce acid value of the oil below 3mg KOH/g which was with different dosages. The next
step was the base catalysed transesterification process which converted the pre-treated oil into biodiesel
and glycerol in the presence of methanol and NaOH at varied reaction conditions. Density of 9.1 lb/gal and
rheological properties; Yield Point (17 Ib/100ft2, 2 Ib/100ft2 and 2 Ib/100ft2), Plastic Viscosity (17cP, 8cP
and 6cP), Gel strength at 10Ȳ (3 Ib/100ft2, 2 Ib/100ft2 and 2 Ib/100ft2) and Gel strength at 10″ (5 Ib/100ft2,
4 Ib/100ft2 and 2 Ib/100ft2) were all determined at temperatures of 80°F, 120°F and 160°F respectively. The
formulated mud showed that biodiesel is a promising synthetic based fluid and has most of its rheological
properties meeting the API standard. Though the initial cost of conditioning biodiesel will be quite high, it
can be offset by its disposal cost as compared to that of diesel.

Introduction
Drilling fluid or drilling mud is a mixture of water, oil, clay and various chemicals. Drilling mud serves many
purposes such as suspending cuttings, controlling pressure, stabilising exposed rocks, providing buoyancy
and lubricate and cool drilling bits. There are three basic types of drilling fluids such as Water Based
Mud (WBM), Oil Based Mud (OBM), and Gaseous/Pneumatic Drilling Fluid (GDF). Adesina et al. (2012)
evaluated the viability of Jatropha, Canola oil, Algae oil and Moringa as alternative to diesel oil in oil-based
drilling mud formulation. The rheological models are critical in drilling fluid study because they are used to
simulate the characteristics of drilling mud under dynamic conditions (Melton and Malone, 1964), with this
knowledge, it is possible to determine the key parameters such as, equivalent circulating density, pressure
drops in the system, and hole cleaning efficiency. Fluids are normally divided into two different groups
2 SPE-193449-MS

according to their flow behaviours: Newtonian fluid model and Non-Newtonian fluid model. The simplest
class of fluids is called Newtonian. Water, mineral oil, gasoline are some examples of such fluids (Peters,
2015). In these fluids, the shear stress is directly proportional to the shear rate. Most drilling fluids are non-
Newtonian fluids, this model does not describe their flow behaviour. The shear stress of a non-Newtonian
fluid is not directly proportional to shear rate and this is why their relationship cannot be described by a
single parameter.
For many years, OBMs have been the preferred drilling mud used in the petroleum industry because of
their better performance over WBMs in borehole stabilization and faster penetration rates. Oil based mud
is a type of drilling mud where the base fluid is a petroleum product such as diesel fuel, mineral oil, or
low toxicity linear olefins and paraffins. Oil based muds are used for several reasons such as to increase
lubricity, enhance shale inhibition (which is critical when drilling horizontal shale formations to be multi-
stage fracked), and greater cleaning abilities with less viscosity (Tharmaraj et al., 2014). Barite is used to
increased system density, and specially treated organophilic bentonite is a primary viscosifier in most oil
based systems. Oil based muds also withstand greater heat without breaking down (Anawe et al., 2014).
The use of this mud has special considerations, these include cost and environmental considerations. Oil
based mud are mostly suitable for High Temperature High Pressure (HTHP) zone (Abduo et al., 2015).
Toxicity refers to the degree to which a chemical is poisonous to plants or animal life in a specific
environment. In many countries that are developing offshore oil and gas resources, discharge permits require
performance of toxicity tests with drilling fluid ingredients and whole drilling fluids. The idea of replacing
diesel OBM with mineral oil based mud was initially derived from toxicity measurements made in U.K
(Stefan, 2016). North-sea countries usually require toxicity testing of individual drilling fluid ingredients;
the Environmental Protection Agency (EPA) requires testing of whole drilling fluids. Toxicity tests are
important for assessing the effects of complex mixtures, such as waste drilling mud on aquatic ecosystems.
From 1970, the Environmental Protection Agency (EPA) and other regulatory bodies of major oil and
gas producing nations are now advocating and imposing increasingly stringent environmental laws and
regulations affecting all aspects of petroleum related operations from exploration, production and refining
to distribution (Adesina et al., 2012).
WBM are the most commonly used of the mud systems and are generally less expensive. The base fluid
may be made up of either fresh water, or salt water. Oil based mud can be formulated with diesel oil, mineral
oil, olefin and paraffins. These olefins paraffins are often referred to as synthetics although some are derived
from distillation of crude oil and some are chemically synthesised from smaller molecules.
Gaseous drilling fluid is actually compressed air or gas that is used instead of water or oil based muds.
Pneumatic systems most commonly are implemented in areas where formation pressures are relatively low
and the risk of lost circulation or formation is relatively high (Anon, 2015).
The development of Synthetics Based Fluids (SBF) provided new options to offshore operators who
depend on the drilling performance of oil based muds to help hold down overall drilling costs and be more
environmentally friendly fluids (Anon, 2015).
Synthetic based mud is a type of drilling mud where the base fluid is synthetic oil. It is also known as
low toxicity oil based mud. Synthetic based fluids are developed out of an increasing desire to reduce the
environmental impacts of offshore drilling operations, but without sacrificing the cost effectiveness of oil
based systems. Synthetic based mud has a continuous phase composed of one or more fluids produced by the
reaction of specific purified chemical feedstock, rather than through physical separation processes (Khan
and Islam, 2007). The SBF material usually represents about 30 to 90 percent of the total volume of the
complete mud (Rushing et al., 1991) and about 20 to 40 percent of the mass of the mud (Kenny, 1993). All
SBF systems contain emulsifiers, wetting agents, thinners, weighting agents, and gelling agents. Relative
proportions of the different ingredients vary, depending on the SBF type and the chemistry, geology, and
depth of the formation being drilled.
SPE-193449-MS 3

Synthetic based fluids and Oil based fluids mostly have the same ingredients. Water usually in the form of
concentrated calcium chloride brine is emulsified in the SBF base materials to increase viscosity. Emulsifiers
are added to SBF to aid in forming and maintaining the inverted emulsion. Barite is used to increase the
weight of the drilling mud, counteracting formation pressure and thus preventing blowout. The amount of
barite added to the mud usually increases as both the depth of the well and the formation pressure increases.
Barite has an extremely low solubility in seawater and so is used frequently as a conservative tracer of the
dispersion and fate of discharged drilling fluids (Neff et al., 2000). There are two generations of SBFs, the
first generation includes esters, ethers, polyalphaolefins and acetal based fluids and the second one includes
linear alphaolefins, linear paraffin and alpha alkyl benzene. There are basically three types of esters; natural
ester, synthetic oleochemical esters, and petrochemical esters. Natural esters were the source of the first
lubricants ever used and they continue to be highly valued in applications such as metalworking fluids, metal
rolling fluids, hydraulic fluids (Eastwood, 2015). They include vegetable crops such as palm oil, vegetable
oil, and animal fats such as tallow (Eastwood, 2015). For natural esters, the base fluids are not based on
petroleum products moreover they are not as costly as the other synthetics.
SBFs have more advantages over WBMs and OBMs. Some of these advantages are to maximize rate
of penetration, increase lubricity in directional and horizontal wells, minimise wellbore stability problems,
such as those caused by reactive shales (Anon, 2015). Also, not all chemically produced SBFs are
biodegradable and economical like the ester (vegetable oils) SBFs. Because of their high biodegradability
and low toxicity, esters are universally recognised as the best based fluids for environmental performance.
One hypothetically available synthetic base is Waste Vegetable Oil (WVO) which is of less usage in Ghana.
In this study, an environmentally friendly synthetic based fluid (biodiesel) has been produced by refining
a waste vegetable oil that came as a by-product from restaurants and fast food joints.

Materials and Methods

Materials Used in the study were:

• Waste Vegetable Oil;

• Methanol (CH3OH) (Analytical grade), Sodium Hydroxide (Analytical grade);

• Isopropyl alcohol (Analytical grade), Phenolphthalein indicator

• Distilled water; Warm Water

• Mass balance, hydrometer, rotational viscometer, blender.

Waste vegetable oil is obtained from cooking and frying. Repeated frying for preparation of food makes
the edible oil no longer suitable for consumption due to high Free Fatty Acid content. Waste oil has
many disposal problem like water and soil pollution, human health concern and disturbance to the aquatic
ecosystem, so rather than disposing it and harming the environment, it can serve as an efficient and cost
effective raw material for production of a synthetic oil based fluid as it is readily available. Vegetable oil
contains saturated hydrocarbon (triglycerides) which consist of glycerol and esters of fatty acids. Used
vegetable oil is a by-product from, fast food joints, restaurants and an operating vegetable oil refinery.
For serving better quality foods, they usually thrown away without any treatment. In some places waste
vegetable oil from restaurants were re-used by the street sellers to fry their foods, this waste oil is termed
the second-used cooking oil and can also be utilized by using it to formulate a synthetic oil based mud.
The chemical and physical properties of waste vegetable oil are different from that of fresh oil since some
changes due to chemical reactions such as hydrolysis, oxidation, polymerization, and material transfer
between food and vegetable oil occur during the frying process (Ridha et al., 2015).
4 SPE-193449-MS

The properties of WVO can change depending on the frying conditions, such as temperature and
frying time. The frying process causes the vegetable oil (triglyceride) to break down to form diglycerides,
monoglycerides and FFAs. The amount of water and heat involved in the frying process also increases
the hydrolysis of triglycerides, therefore it causes a growth of the free fatty acids in the WVO. Moreover
due to oxidation and polymerisation reactions, there is an increase in the viscosity and the saponification
number of the WVO when compared with the original oil. The presence of water in the WVO samples often
lead to hydrolysis. Both hydrolysis and saponification reactions cause low biodiesel yield and high catalyst
consumption (Wang, 2014).

Methods Used
The following steps 1 to 7 were used to undertake this study:
1. Determination of Density of WVO
The density of the Waste vegetable oil was determined by using the hydrometer.
2. Determination of Acid Number of WVO
The acid value was determined by titration of the sample using KOH as the titrant solution and
phenolphthalein as the indicator. The titration process was stopped when the solution turned into pink
colour. The acid value (AV) was calculated using the equation 1:

(1)

Where: 56.1 - molecular weight of the solution employed for titration (g/mol), VKOH - consumption
during titration (ml), CKOH (mol/l) - concentration of the titration KOH solution, m - weight (g) of
the sample.
3. Pre-Treatment of Waste Vegetable Oil by Filtration
A titration process was carried out to determine the amount of catalyst required for the reaction
as well as the amount of catalyst required to neutralise the Free Fatty Acids (FFA). The oil was also
filtered to remove any chunks of food particles passing the oil through a cotton cloth.
4. Pre-Treatment of Waste Vegetable Oil by Esterification Reaction
100 ml of waste vegetable oil was poured into the reactor, and heated at 60 °C. Methanol and H2SO4
were mixed before the reaction. The oil was heated to the desired temperature before the addition
of methanol and H2SO4 mixture. The mixture was kept to settle for 6 hours resulting in two distinct
liquid phases. The methanol-water fraction at the top was removed using separating funnel.
5. Alkaline Catalysed Transesterification Reaction
The pre-treated oil was heated up to 60 °C. 1 %w/v Sodium Hydroxide (NaOH) was dissolved in
20 % of methanol to oil volume ratio under vigorous stirring to form a methoxide, and then added to
the pre-treated waste vegetable oil. The mixture was again heated 60 °C to and stirred for 30 minutes.
After that, the solution was kept to settle 16 hours to a separate. The bottom glycerol layer and the
top methyl ester (crude biodiesel) layer were then separated.
6. Purification of Biodiesel
Biodiesel was separated and washed by distilled water for removal of minor impurities. The washed
biodiesel was heated to remove any moisture present. The purification of crude biodiesel (methyl
esters) can be done by treating with Na2SO4 to remove water and also by using activated carbons
produced from spent tea waste which result in higher yield of product and better fuel properties
compared to the conventional methods of water washing and use of silica gel.
SPE-193449-MS 5

Figure 1—A Separation of Biodiesel and Glycerol

Figure 2—Washed Biodiesel

Mud Formulation
The base oil used for the experiment was biodiesel which was produced from waste vegetable oil. The
materials and respective quantities used to formulate the mud are represented in Table 1.

Table 1—Materials Used and their required Quantities

Materials Quantity

Organophilic clay (g) 6

Oil (Biodiesel) (ml) 315

Water (ml) 35

Primary Emulsifier (ml) 5

Secondary Emulsifier (ml) 2

Calcium chloride (g) 9

Barite (g) 78

Lime (g) 6

Procedures for mud sample preparations are as follows;

i. Base fluid (Biodiesel) is measured into the mixing vessel;
ii. Add primary emulsifier and secondary emulsifier as required;
iii. After five minutes of mixing, add the lime;
6 SPE-193449-MS

iv. Calcium chloride was weighed and poured in water to obtain a brine solution;
v. Add the brine;
vi. Add organophilic clay as required;
vii. Mix for about ten minutes to ensure a good emulsion is formed; and
viii. Add weighting materials as required for the desired density was added.

Determination of the Rheological Properties of Mud Sample

The rheological properties (Apparent Viscosity (AV), Plastic Viscosity (PV), and Yield Point (YP)) of the
mud sample were calculated from the viscometer dial readings presented in the following equations:
(2)

(3)

(4)

Results
The target acid value suggested is less than 3 mg KOH/g (roughly 1 % FFA) in order to proceed to the
alkali-catalysed transesterification. An experiment was carried out to vary the effects of various alcohol
and catalyst concentrations on the acid value during the esterification process as well as their effects on the
biodiesel yield after the transesterification reaction.
The following Figures (3-5) and Table 2 presents the observation made during the experiment.

Figure 3—Influence of Methanol Amount on Acid Value by Using 0.5 % of Sulfuric Acid-to-Oil Volume Ratio
SPE-193449-MS 7

Figure 4—Influence of Methanol Amount on Acid Value by Using 1 % of Sulfuric Acid-to Oil Volume Ratio

Figure 5—Influence of Methanol Amount on Acid Value by Using 1.5 % of Sulfuric Acid-to Oil Volume Ratio

Table 2—Effect of Sulfuric Acid on Acid Value of Waste Vegetable Oil

Volume of Sulfuric Acid (ml) Volume of Methanol to Oil Ratio (ml) Acid Value of Pretreated
Oil (mg KOH/g- oil)

0.5 40:100 22.42

0.5 50:100 16.24

0.5 60:100 14.82

0.5 70:100 13.59

1.0 40:100 8.44

1.0 50:100 8.02

1.0 60:100 3.82

1.0 70:100 2.22

1.5 40:100 6.73

1.5 50:100 4.11

1.5 60:100 2.86

1.5 70:100 2.91

8 SPE-193449-MS

Mud sample
Table 3 and table 4 shows the properties and physiochemical properties of waste vegetable in its raw state
and produced biodiesel. Also Table 5 presents the viscometer readings of the mud samples at 80 °F, 120 °F
and 160 °F which were used to calculate for the rheological properties (Apparent Viscosity (AV), Plastic
Viscosity (PV), and Yield Point (YP)) in equation 2, 3 and 4 respectively. Figures 6-7 and table 6 shows the
results of the experiment carried out on the 10 seconds and 10 minutes gel strength of the mud sample at 80
°F, 120 °F and 160 °F respectively. The rheological properties of the mud sample are presented in table 7.

Table 3—Properties of Waste Vegetable Oil

Properties Values obtained

Acid Value 64.82 mg KOH/g- oil

Free Fatty Acid 32.41 %

Density @ 15 °C 0.88 g/cm3

Table 4—Physiochemical Properties of Biodiesel Derived from Waste Vegetable Oil

Parameter Unit Waste Vegetable Oil Biodiesel

Viscosity @40 °C mm2/s 35.4 3.9

Density @15 °C g/cm3 0.91 0.88

Flash point °F – 132

Pour point °F – 11.4

Ester conversion % 85

Table 5—Viscometer Readings of Mud Sample at 80 °F, 120 °F and 160 °F

Dial Readings Temperature (° F)

(RPM) 80 ° F 120 ° F 160 ° F

600 34 20 16

300 17 12 10

200 12 9 7

100 7 6 4

6 4 3 2

3 2 2 2

Table 6—Gel strengths of Mud Sample at 80 °F, 120 °F and 160 °F

Temperature (° F) Gel strength @ Gel strength @

10′ (Ib/ 100ft2) 10″ (Ib/ 100ft2)

80 3 5

120 2 4

160 2 2
SPE-193449-MS 9

Table 7—Rheological properties of mud sample

Rheological Yield strength, lb/1000ft2 Plastic viscosity, cp Gel 10 seconds strength, lb/1000ft2
properties 10 minutes

80 °F 120 °F 160 °F 80 °F 120 °F 160 °F 80 °F 120 °F 160°F 80 °F 120 °F 160°F

Values x 17 2 2 17 8 6 3 2 2 5 4 2

Figure 6—10 Seconds Gel Strength of Mud Sample at 80 °F, 120 °F and 160 °F

Figure 7—Minutes Gel Strength of Mud Sample at 80 °F, 120 °F and 160 °F

Density of mud was determined at room temperature (80 °F). API recommends a density of 7.5 lb/gal to
over 22 lb/gal. The result obtained from the density measurement using hydrometer was 9.1 lb/gal. Figure
8 shows the behaviour of the formulated mud from the plot of the recorded shear stress against shear rate.
10 SPE-193449-MS

Figure 8—Shear stress against Shear rate plot

Discussion
Due to the high free fatty acids content in waste frying oil, the transesterification reaction of the oil can risk
the soap formation in the presence of sodium hydroxide. To avoid saponification reaction, the pretreatment
of the oil by the esterification reaction with sulfuric acid in the presence of methanol was required to reduce
the Free Fatty Acids (FFA) to the limit necessary to achieve the transesterification reaction. The results
presented in Table 2 indicate that the dosage of sulfric acid during the esterification process affected the
free fatty acid content.
The effect of quantity of methanol on acid value in waste vegetable oil after esterification process by
using 0.5% v/v, 1% v/v and 1.5 % v/v of sulfuric acid to oil volume ratios is shown in the Figures (2- 4).
High amount of methanol was required to reduce the acid value of the pretreated oil to 2.22 mg KOH/g.
The lowest acid value was obtained with 70 ml methanol to oil ratio. Figures 3 and 4 shows that with 60
ml and 70 ml of methanol the acid values were lower than 5 mg KOH/g-oil. The results that the acid values
decreased gradually with an increasing amount of methanol.
The gel strength is another important drilling fluid property, as it demonstrates the ability of the drilling
mud to suspend drilled cuttings and weighting material when mud circulation is ceased. API recommends
ranges of 3 – 20 (lb/100 ft2) and 8 – 30 (lb/100 ft2) for 10 seconds and 10 minutes gel strength respectively.
The mud formulated passed 10 seconds gel strength at 80 °F and failed both 10 seconds and 10 minutes gel
strength at 120 °F and 160 °F gel strength readings as shown in table 6 and figure 5 and 6 respectively.
The viscosity readings of the mud samples in table 5 at 80 °F, 120 °F and 160 °F respectively shows that,
the mud sample was noticed to be decreasing with an increase in temperature.
The rheological properties of the mud sample as indicated in table 7 shows that the Yield Point was
(17 Ib/100ft2, 2 Ib/100ft2 and 2 Ib/100ft2), Plastic Viscosity (17 cP, 8cP and 6 cP), Gel strength at 10’ (3
Ib/100ft2, 2 Ib/100ft2 and 2 Ib/100ft2) and Gel strength at 10" (5 Ib/100ft2, 4 Ib/100ft2 and 2 Ib/100ft2) were
all determined at temperatures of 80 °F, 120 °F and 160 °F respectively. According to the rheological model
of the mud sample as seen in figure 7, it can be said that the shear rate increases with an increase in the
shear stress.
Since the rheological properties of the mud sample were in the range of the API recommendation, it can
be said that biodiesel based mud possesses a great chance of being among the feasible replacements for
oil based muds.
SPE-193449-MS 11

Conclusion
• Biodiesel can be produced from waste vegetable oil with high free fatty acid using the two stage
process; esterification and transesterification.
• The results of the tests carried out indicated that biodiesel synthetic based muds possess great
chances of being among the feasible replacements for oil based muds.

Acknowledgement
I would like to appreciate the University of Mines and Technology (UMaT) and Total Petroleum (Tarkwa
Mine Depot) for all their supports.

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