Citation: Enyiegbulam ME, Iheaturu NC.

Effect of Spent Oil Base Drilling

Mud Solids on the Mechanical Properties of UPR Composites. Journal of
Polymer Engineering. 2007;27(2):149–63. Doi:10.1515/polyeng.2007.27.2.149
http://www.degruyter.com/view/j/polyeng.2007.27.2/polyeng.2007.27.2.149/po
lyeng.2007.27.2.149.xml

EFFECT OF SPENT OIL BASE DRILLING MUD SOLIDS ON THE

MECHANICAL PROPERTIES OF FILLED UPR COMPOSITES

*Enyiegbulam, M. E. and Iheaturu, N. C.

Dept. of Polymer & Textile Engineering, Federal University of Technology, Owerri.

Imo, Nigeria
enyiegbulaman@yahoo.com, nnamdi234@yahoo.com

ABSTRACT

Drilling mud solid content was recovered from spent oil base drilling mud (SOBM)
samples collected from a rig site in Bonny Island, Rivers State, Nigeria. The mud solids (clays)
were sieved into different particle sizes and calcined at 900°C for 2hrs, then treated with 40%
ethylamine at 120°C.
Solids in spent oil base drilling mud constitute about 55.65% per 100mls. Particle size
analysis show that recovered spent mud sample contains about 77.48% of particles with size
less than 300µm.
The samples were complexed into unsaturated polyester (UPR) resin composite using the
in-situ formation technique. Tests carried out on the samples show that 63µm, 75µm, 100µm,
300µm and 425µm filled composites gave modulus of 1666.67 x 106 Nm-2, 312.5 x 106 Nm-2,
156.25 x 106 Nm-2, 125 x 106 Nm-2 and 104.2 x 106 Nm-2 respectively. Ultimate strength was
39.38 x 106 Nm-2, 43.75 x 106 Nm-2 for 63µm and 75µm filled composites respectively and
remained 37.5 x 106 Nm-2 for 100µm, 300µm and 425µm filled composites. UPR composite
filled with 63µm size SOBM solids gave material with the highest modulus, resulting to
improved tensile properties.

Keywords: Spent Oil Base Drilling Mud (SOBM), Clay, Calcination, Unsaturated Polyester
Resin (UPR), Methyl Ethyl Ketone Peroxide (MEKP), Nanocomposites, Microcomposites.

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1.0 INTRODUCTION

A nanocomposite comprises an inorganic phase in the nanosize dimension and polymer

matrix /1/, with the result that the inorganic phase provides strength, dimensional stability,
toughness, opacity and high temperature resistance. The inorganic component otherwise called
“filler” or “reinforcement” maybe a 3D framework as zeolites, 2D layered materials as clays,
metal oxides, metal phosphates, chalcogenides or a one dimensional and zero dimensional
material as molybdenium selenate (Mo3Se-)n /2/. Nanoparticles such as precipitated silica
(Motomatsu et al, 1997) /3/, silica-titania oxides synthesized by sol gel process (Wen and
Mark, 1994) /4/, Silica beads (Pu et al, 1996) /5/ and rigid polymer colloids (Rukenstein and
Yaun, 1997) /6/, have been used in the production of polymer nanocomposites. The organic
component is either a thermoplastic or thermoset material. The two dissimilar materials are
mixed at nanoscale to produce intercalated, exfoliated or conventional hybrid composites /7/.
In-situ technique for formation of nanocomposites has been elucidated by Carrado and Xu,
1998 /8/. They used in-situ hydrothermal crystallization of silicate layers in an aqueous
polymer gel to form composites. Conventional stress-strain curves are calculated based on the
original cross-sectional area with stress varying directly with strain. Since the cross sectional
area decreases as tensile force is applied, the true stress and true strain response of a material is
based on its actual cross-sectional area /9, 10/, giving higher values for true stress and true
strain. Equations 1 and 2 below give values for true stress and true strain from nominal or
conventional stress-strain values.

εT = εlog = ln (1 + ε) (1)

σT = σ (1 + ε) (2)

where: εT = True strain, ε = Nominal strain

σT = True stress, σ = Nominal stress

In essence, the aim of microscopic reinforcement in this study is to investigate the effect of
calcined spent oil base drilling mud (SOBM) solids on the mechanical properties of filled
unsaturated polyester (UPR) composites.

2.0 MATERIALS AND METHODS

2.1 Sample Collection And Preparation

Spent oil base drilling mud samples were obtained from a rig site in Bonny Island, Rivers

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State, Nigeria. The samples were carefully collected in 2 litres polyethylene bottles. All
reagents used for this study were of analytical grade and conformed to the specifications of the
Committee on Analytical Reagents of the American Chemical Society (ACS).
Sieves used for the particle size analysis conformed to specification E11 (American
National Standard). The nest of sieves varies in opening size by the ratio of √2:1. Sieve
designation conformed to ASTM E11 – 81, BS 410 1986.

2.2 Extraction of SOBM Solid Content

SOBM solid content was extracted from its liquid base (mineral oil, based on asphaltenes)
using a metallic evaporating dish on an open flame. The sample was extracted by completely
burning off the highly inflammable but yet toxic oil base liquid. The recovered solids which
now appear in dark brown coloured crumbs was crushed in a ceramic mortar and sieved into
various sizes as indicated in Table 1.

Table 1
Nest of sieves and sizes used for this study
Sieve No. Size Marked Sieve
8 2.36mm
12 1.70mm
16 1.18mm
20 850μm 
30 600μm 
40 425μm 
50 300μm 
70 212μm
100 150μm
140 100μm 
200 75μm 
212 63μm 
The marked sieves were the ones used for this study.

2.3 Sieving
Dry sieving method was carried out in accordance with the standard test method for sieve
analysis and water content of refractory materials as enumerated in ASTM C 92 – 76. Dry
sieving was carried out mechanically and the quantity of material retained on each sieve was
determined by weighing, to the nearest 0.01g.

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2.4 Calcination
SOBM sample was calcined in a laboratory size potclay kiln: model no.; GK 4 3215, with
maximum permissible temperature of 1200°C. Heating was continuous and increased gradually
to maximum required temperature of 900°C. The temperature was maintained continuously for
2hrs.

2.5 Chemical Composition of SOBM Solids

The method used to determine chemical composition, as elucidated in ASTM D3562 –
3568, APHA 3111B, 3111D and CAEM, was adopted to determine percentage composition of
potassium (K+) and potassium oxide, calcium (Ca2+) and calcium oxide, silicon (Si4+) and
silica, sodium (Na+) and sodium oxide, magnesium (Mg2+) and magnesium oxide, iron (Fe3+)
and iron III oxide, aluminum (Al2+).

2.6 Incorporation of Calcined Material into UPR

The sample was complexed into unsaturated polyester (UPR) composite. Before
incorporation into UPR, the calcined material was treated with 40% ethyl amine solution and
dried in the oven at 120°C for 30mins. The in-situ method of formation of polymer composites
was used for this research. The mixture of resin, filler and additives was poured into a wooden
mould to cast a dumb bell shaped material which dimensions is as shown in Figure 1. Cure
temperature was 32C (under sunlight). The effects of particle size on hardness and tensile
strength were noted. Material thickness = 0.4mm.

Table 2
Formulation for UPR composite

S/No. Item 1 5 3 2 4 Unfilled

1. 5g of material (m) 425 300 100 75 63 -
2. UPR (50mls)      
3. MEKP (2 drops)      
Cobalt naphthanate (1 
4. drop)     
Wetting agent (40%
5. Ethyl amine solution)      -

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Fig. 1: Dog-bone UPR composite (All dimensions in mm)

2.7 Tests For Tensile Properties

The material was subjected to tensile stress using the MONSANTO tensometer according
to ISO 527, ASTM D-638. At a constant rate of loading, the material was pulled until a point
of failure. The graph of continuous loading against extension was traced on a graph sheet.

2.8 Tests For Hardness Of UPR Composite

The Rockwell hardness test was carried out on the filled and unfilled UPR composite
material. This test was carried out to investigate the effect of particle size on material hardness.
Indentation test instrument according to ASTM D-2240 was used. Rockwell B, with ball size
1.58mm (1/16in) indentor, 10kg minor / 100kg minor was used to test the filled and unfilled
plastic composite material.

3.0 RESULTS AND DISCUSSIONS

3.1 Solid Content Extraction

The results of solid content recovered from SOBM are shown below as follows:

Table 3
Result of mud solids recovery

Wt. of Percentage Wt. of Percentage

Wt. of
recovered solid liquid liquid
Beaker SOBM
solids content content content
(grams)
(grams) per 100mls (g) (%)
A 127.12 82.05 66.91 45.07 35.45
B 125.60 64.03 50.98 61.57 49.02
C 123.11 63.07 51.23 60.04 48.77
Average 125.28 69.72 55.65% 55.56 44.35%

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The results of the mud solids extraction show that out of 125.28g (100%) of spent drilling
mud collected from the rig site, mud solids constitute about 69.72g or 55.65% of the recovered
spent mud sample. Liquid content, which includes oil and water, constitutes 55.56g or 44.35%
of the spent drilling mud sample. More than half of the spent drilling mud sample is composed
of mud solids. High solid content in drilling mud causes stock pipe during drilling and is a
health risk both to the operatives on the rig site and to the environment to which spent mud is
to be disposed of.

3.2 Results of Sieving and Particle Size Analysis

Particle size distribution of the recovered SOBM sample was determined by calculating the
weight fraction of each particle size aggregate based on the total weight of 550.88g.

Table 4
Particle size distribution

Sample
size (m) 63 75 100 150 300 425 600 850 850 1000 Total

Wt. of
sample 2.47 34.9 22.88 35.06 331.51 7.18 87.57 7.2 7.2 22.11 550.88
(grams)

Table 5
Particle size analysis

Weight Weight Cumulative

Sample size(m) Percentage (%)
(g) fraction Frequency
0 – 63 2.47 0.0045 0.45 0.45
64 – 75 34.9 0.0634 6.34 6.78
76 - 100 22.88 0.0415 4.15 10.94
101 – 150 35.06 0.0636 6.36 17.30
151 – 300 331.51 0.6018 60.18 77.48
301 – 425 7.18 0.0130 1.30 78.78
426 – 600 87.57 0.1590 15.90 94.68
601 – 850 7.2 0.0131 1.31 95.99
851 – 1000 22.11 0.0401 4.01 100.00
550.88 1.0000 100.00

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Particles of size between 0 to 63m, represent 0.45% by weight of recovered SOBM, 64 –

75µm (6.34%), 76 – 100µm (4.15%), 101 – 150µm (6.36%), 151 – 300µm (60.18%), 301 –
425 (1.30%), 426 – 600µm (15.90%), while the rest or very coarse particles of size between
601 – 1000µm, represent 5.32%.
The results of the particle size distribution show that recovered spent mud sample contains
about 77.48% of particles with size less than 300μm.

3.3 Chemical Composition Of Calcined SOBM Solids

Table 6 shows percentage composition of heavy metals and their oxides in the calcined
SOBM solids.

Table 6
Results of IR and atomic absorption spectroscopy

Chemical Calcined Chemical

Calcined SOBM %
component SOBM % composition component
solids composition
(mg/kg) solids (mg/kg)

1 Silicon 443 0.96 Silica (SiO2) 948.00 1.45

Aluminium
2 Aluminium 215 0.47 oxide (Al2O3) 406.00 0.62

Calcium oxide
3 Calcium 43,910 95.01 (CaO) 61,439.00 94.26

Magnesium
4 Magnesium 341 0.74 oxide (MgO) 565.00 0.87

Potassium oxide
5 Potassium 136 0.29 (K2O) 164.00 0.25

Sodium oxide
6 Sodium 253 0.55 (Na2O) 341.00 0.52

Iron III oxide

7 Iron 920 1.99 (Fe2O3) 1,315.00 2.02

TOTAL TOTAL
46,218.00 100.00 65,178.00 100.00
(mg/kg) (mg/kg)

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3.4 Results of Tensile Test on Filled UPR Composite

The following results were obtained from the tensile test carried out on the UPR samples.

Table 7
UPR 1 (Unfilled)
Nominal
Force Lo - L log strain True stress
Area (m2) stress Lo (mm) Strain () 1+
(N) (mm) ln(1+) σT=σ(1+)
(Nm-2)

0 0.000016 0 50 0.00 0.000 1.000 0.000 0

200 0.000016 12500000 50 3.00 0.060 1.060 0.058 13250000
400 0.000016 25000000 50 5.00 0.100 1.100 0.095 27500000
440 0.000016 27500000 50 7.00 0.140 1.140 0.131 31350000
500 0.000016 31250000 50 9.00 0.180 1.180 0.166 36875000
600 0.000016 37500000 50 13.00 0.260 1.260 0.231 47250000
600 0.000016 37500000 50 16.50 0.330 1.330 0.285 49875000
560 0.000016 35000000 50 20.00 0.400 1.400 0.336 49000000

Table 8
UPR 4 (63 μm)
Nominal stress Lo - L log strain True stress
Force (N) Area (m2) Lo (mm) Strain () 1+
(Nm-2) (mm) ln(1+) σT=σ(1+)
0 0.000032 0 50 0 0.000 1.000 0.000 0
200 0.000032 6250000 50 0.20 0.004 1.004 0.004 6275000
300 0.000032 9375000 50 0.45 0.009 1.009 0.009 9459375
420 0.000032 13125000 50 0.75 0.015 1.015 0.015 13321875
600 0.000032 18750000 50 0.95 0.019 1.019 0.019 19106250
700 0.000032 21875000 50 1.35 0.027 1.027 0.027 22465625
900 0.000032 28125000 50 1.75 0.035 1.035 0.034 29109375
1000 0.000032 31250000 50 2.00 0.040 1.040 0.039 32500000
1200 0.000032 37500000 50 2.30 0.046 1.046 0.045 39225000
1260 0.000032 39375000 50 2.60 0.052 1.052 0.051 41422500

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Table 9
UPR 2 (75 μm)
Nominal stress Lo - L log strain True stress
Force (N) Area (m2) Lo (mm) Strain () 1+
(Nm-2) (mm) ln(1+) σT=σ(1+)
0 0.000032 0 50 0 0.000 1.000 0.000 0
200 0.000032 6250000 50 1.00 0.020 1.020 0.020 6375000
400 0.000032 12500000 50 2.00 0.040 1.040 0.039 13000000
600 0.000032 18750000 50 4.50 0.090 1.090 0.086 20437500
900 0.000032 28125000 50 7.00 0.140 1.140 0.131 32062500
1200 0.000032 37500000 50 10.00 0.200 1.200 0.182 45000000
1360 0.000032 42500000 50 15.00 0.300 1.300 0.262 55250000
1400 0.000032 43750000 50 17.20 0.344 1.344 0.296 58800000

Table 10
UPR 3 (100 μm)
Nominal stress Lo - L log strain True stress
Force (N) Area (m2) Lo (mm) Strain () 1+
(Nm ) -2
(mm) ln(1+) σT=σ(1+)
0 0.000032 0 50 0.00 0.000 1.000 0.000 0
200 0.000032 6250000 50 2.00 0.040 1.040 0.039 6500000
400 0.000032 12500000 50 3.20 0.064 1.064 0.062 13300000
600 0.000032 18750000 50 7.50 0.150 1.150 0.140 21562500
700 0.000032 21875000 50 13.00 0.260 1.260 0.231 27562500
800 0.000032 25000000 50 16.00 0.320 1.320 0.278 33000000
860 0.000032 26875000 50 18.50 0.370 1.370 0.315 36818750
900 0.000032 28125000 50 22.50 0.450 1.450 0.372 40781250
980 0.000032 30625000 50 24.50 0.490 1.490 0.399 45631250
1120 0.000032 35000000 50 27.90 0.558 1.558 0.443 54530000
1200 0.000032 37500000 50 30.00 0.600 1.600 0.470 60000000
1200 0.000032 37500000 50 32.00 0.640 1.640 0.495 61500000
1200 0.000032 37500000 50 39.50 0.790 1.790 0.582 67125000

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Table 11
UPR 5 (300 μm)
Nominal log
Force Area Lo - L Strai True stress
stress Lo (mm) 1+ strain
(N) (m2) (mm) n () σT=σ(1+)
(Nm-2) ln(1+)
0 0.000032 0 50 0.00 0.000 1.000 0.000 0
200 0.000032 6250000 50 2.50 0.050 1.050 0.049 6562500
300 0.000032 9375000 50 4.50 0.090 1.090 0.086 10218750
400 0.000032 12500000 50 6.50 0.130 1.130 0.122 14125000
500 0.000032 15625000 50 9.00 0.180 1.180 0.166 18437500
600 0.000032 18750000 50 16.00 0.320 1.320 0.278 24750000
700 0.000032 21875000 50 19.00 0.380 1.380 0.322 30187500
800 0.000032 25000000 50 24.00 0.480 1.480 0.392 37000000
900 0.000032 28125000 50 27.50 0.550 1.550 0.438 43593750
1000 0.000032 31250000 50 31.00 0.620 1.620 0.482 50625000
1100 0.000032 34375000 50 33.50 0.670 1.670 0.513 57406250
1140 0.000032 35625000 50 37.50 0.750 1.750 0.560 62343750
1200 0.000032 37500000 50 44.50 0.890 1.890 0.637 70875000

Table 12
UPR 6 (425 μm)
Force Nominal stress Lo - L log strain True stress
Area (m2) Lo (mm) Strain () 1+
(N) (Nm-2) (mm) ln(1+) σT=σ(1+)

0 0.000032 0 50 0.00 0.000 1.000 0.000 0

200 0.000032 6250000 50 3.00 0.060 1.060 0.058 6625000
300 0.000032 9375000 50 5.00 0.100 1.100 0.095 10312500
400 0.000032 12500000 50 7.00 0.140 1.140 0.131 14250000
500 0.000032 15625000 50 9.00 0.180 1.180 0.166 18437500
600 0.000032 18750000 50 14.00 0.280 1.280 0.247 24000000
700 0.000032 21875000 50 18.50 0.370 1.370 0.315 29968750
800 0.000032 25000000 50 24.60 0.492 1.492 0.400 37300000
900 0.000032 28125000 50 27.50 0.550 1.550 0.438 43593750
1000 0.000032 31250000 50 32.50 0.650 1.650 0.501 51562500
1100 0.000032 34375000 50 35.00 0.700 1.700 0.531 58437500
1150 0.000032 35937500 50 37.50 0.750 1.750 0.560 62890625
1200 0.000032 37500000 50 41.50 0.830 1.830 0.604 68625000

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A comparative analysis of mechanical properties of the filled and unfilled composite material
is shown in Figure 2.

50000000

45000000

40000000

35000000
Nominal Stress (Nm -2)

30000000

25000000 63 microns

75 microns
20000000
100 microns
15000000
300 microns
10000000 425 microns

5000000 Unfilled

0
0.000 0.100 0.200 0.300 0.400 0.500 0.600 0.700 0.800 0.900 1.000

Strain

Fig. 2: Plot of stress against strain for calcined SOBM filled and unfilled
UPR composite

From Figure 2, UPR filled with 63m SOBM filler is a brittle material because abrupt
fracture occurred at very low strains (elastic limit; 0.02mm) and relatively high strength. Yield
strength is undefined using the nominal stress strain curve.
UPR filled with 75m SOBM filler is hard and tough with abrupt yielding at very high
strength. This material has a high modulus of 312.5 x 10 6 Nm-2 and high breaking strength of
43.75 x 106 Nm-2.
UPR filled with 100m, SOBM filler have very low yield. The properties include; elastic
limit, 0.04mm; modulus, 156.25 x 106 Nm-2; ultimate strength, 37.5 x 106 Nm-2; breaking
strength, 37.5 x 106 Nm-2.
UPR filled with 300m and 425m, have similar curve. However, properties of composite
filled with 425m came very close to properties of unfilled UPR material, with very low yield
strength of 9.375 x 106 Nm-2, modulus (125 x 106 Nm-2 and 104.2 x 106 Nm-2 respectively),
and elastic limit (0.03 to 0.04mm respectively). The 2 materials exhibited high resilience
similar to that of a rubbery material, with elongation at break of 44.5 and 41.5mm respectively.

3.5 Design Considerations

3.5.1 The effect of particle size on tensile properties of UPR SOBM filled composite
Table 13 shows the effects of calcined SOBM filler particle size on sample tensile
properties. Such properties include; modulus of elasticity, breaking strength, elongation at
break, elastic limit and ultimate strength.

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Table 13
Significant material mechanical properties
Material
S/No. Material property with different particle sizes
Property

Filler particle
1 size (microns) 0 63 75 100 300 425

Modulus of
2 Elasticity 200.00 1666.667 312.50 156.25 125.00 104.20
(x 106 Nm-2)
Breaking
3 strength 35.00 39.375 43.75 37.50 37.50 37.50
(x 106 Nm-2)

Elongation at
4 break (mm) 20.00 2.60 17.20 39.50 44.50 41.50

Elastic limit
5 (mm) 0.02 0.003 0.02 0.04 0.03 0.04

Ultimate
6 strength 38.00 39.375 43.75 37.50 37.50 37.50
(x 106 Nm-2)

Yield Strength
7 (x 106 Nm-2) 25.00 13.125 18.75 12.50 9.375 9.375

SOBM filler particle size affects composite breaking and ultimate strength in a similar way,
except for unfilled material. 75m filled composite gave the highest breaking and ultimate
strength. However, both properties remained constant at filler sizes 100, 300 and 425m.
Elongation at break increased rapidly between composites filled with 63m and 100m,
while modulus of elasticity and yield strength decreased rapidly with increase in filler size,
except in materials filled with 75m filler size where there was a sharp increase in material
properties.
Unfilled UPR, gave a very poor material with low modulus, low breaking strength, low
ultimate strength and moderate elongation at break.

4.7.2 Rockwell hardness test on UPR filled composite

The results of the Rockwell B hardness tests carried out on the filled and unfilled composite
material are shown below.

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Table 14
Results of Rockwell “B” hardness of filled and unfilled UPR composite

Particle size
Sample ID HR"B"
(micrometer)
Unfilled (1) 0 51
Filled (4) 63 78
Filled (2) 75 82
Filled (3) 100 86
Filled (5) 300 88
Filled (6) 425 93

Rockwell hardness “B” of calcined SOBM filled UPR composites increased with filler size.

5.0. CONCLUSION

The true stress-strain and nominal stress-strain values for composites filled with 63 and
75m particles indicate that, stress was somewhat evenly distributed between the matrix and
the inorganic SOBM filler. For the other composite materials, far apart values of true stress-
strain and nominal stress-strain curves show that stress is not evenly distributed between UPR
matrix and inorganic material. Values for modulus, ultimate strength, yield strength and
breaking strength for 300m and 425m filled composites gradually tend towards properties of
unfilled material. Further reduction of calcined SOBM filler size would give a material whose
true stress-strain and nominal stress-strain properties are equal values for UPR filled
composite.

ACKNOWLEDGEMENT

My profound appreciation goes to Mr. Tony Ododoiye, Invar Chemicals and Engineering
Co. (Nig.) Ltd., Aba, Nigeria and to the technologists of Institute of Erosion Studies, Dept. of
Materials / Metallurgical Engineering and Dept. of Polymer / Textile Engineering, Federal
University of Technology, Owerri, Imo, Nigeria.

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Fig. 1: Dog-bone UPR composite (All dimensions in mm)

Fig. 2: Plot of stress against strain for calcined SOBM filled and unfilled UPR composite.

162