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Evaluation study for lubricant grease prepared from Iraqi bentonite

Article  in  Journal of the Balkan Tribological Association · January 2013

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Journal of the Balkan Tribological Association Vol. 19, No 2, 294–301 (2013)

Lubrication – grease from Iraqi bentonite

Evaluation Study for Lubricant Grease Prepared

from Iraqi Bentonite

Mohammad Jamil Abd-Alghani

University of Sallah- Al-Din, College of Basic Education, Arbil, Republic of Iraq

Abstract

The present research is directed toward preparation of bentonite grease from Iraqi
bentonite by converting the hydrophilic bentonite into organophilic in order to
ensure depression into the base stock oil. Quaternary ammonium chloride and
bromide with 8 carbon atoms as a minimum requirement were used. Results indi-
cate that the chloride salt was more efficient than bromide salts, and the optimum
percent of salt added was 30% which resulted in calcium ion exchange.
Two types of base oil stocks were used: stock 60 and stock 150 with a vis-
cosity of 67.25 and 414.73 cSt, respectively. Methanol (wt. 1%) was used as a dis-
persion agent at 40 C° to yield homogeneous mixture and air bubbles free. Wax
(wt. 7%) was added to prevent the isolation between base oil and thickener, 5%
(by vol.) asphalt was used with the base oil stock 150 which gave a grease with a
viscosity of (575 cSt) and drop point of 250 C°.
Different bentonite percentages were used to prepare grease, the results
showed that increasing the bentonite percentage and viscosity caused in:
1.  decreasing the penetration point;
2.  increasing the drop point and resistance to grease washout.
Keywords: bentonite, penetration, drop point.

aims and background

Grease is a complex lubricant which consists of base oil (65–95%), additives (0–
10%) and thickener (3–30%) (Ref. 1), which forms a network that acts as reservoir
for the oil. Most grease thickeners are lithium, calcium, sodium and barium or
aluminum soaps, non soap are silica, clays and certain organic compounds which
are also used as dye stuffs2. The soap gives the grease a semisolid appearance and
enables lubrication in applications where a continuous supply of oil is not possi-
ble. In 80–90% of all rolling element bearings, grease is the preferred lubricant, it
is easy to apply and it does not leak easily. Low friction is obtained after an initial
294
running period where the grease is redistributed through the bearing and moves
to the sides of the running. The grease is retained in the bearing using a simple
shield or seal bandit continuously supplies oil to the contact surfaces for lubrica-
tion3. This mechanism where oil is slowly released from the grease is called oil
bleeding and is of great importance for bearing performance and reliability.
In general, any lubricating fluid gelled by means of suitable thickeners to
form lubricating grease. In practice, mineral oils are almost exclusively used4.
A physical examination of soap thickened grease will show it to be of fibrous
nature. The fiber structure is responsible for thickening the oil to form grease, will
depend predominantly on the type of soap used and the method of manufacturing.
The fiber length may be short which results in smooth buttery texture. Alterna-
tively, the fiber length may be long which will result in stringy type texture5.
Various types of chemically or physically modified clays have been sug-
gested as thickeners for lubricating fluids. Most of these gelling agents are de-
rived from natural clays. An organophilic bentonite was the first thickener to
have widespread in the manufacture of lubricating grease6. In 1977, it was stated
that organophilic bentonite thickened lubricants usually have no dropping point
and they will burn rather than melt. As a result, in 1985, it was recommended that
organoclay greases should be milled to enhance their properties such as gallant
efficiency, homogeneity, consistency, and bleed resistance6,7.
Dialkyl benzene thickened with bentonite has been used in equipment in-
tended for use in the Arctic, characteristics and conclusions are drawn as their
suitability. According to these characters for various applications, it was reported
that universal grease has been formed with bentonite and synthetic hydrocarbon
for military use [4].
Bentonite-based greases are characterised by high dropping point, good re-
tention to metal and high water resistance. These greases have been used for lu-
brication of many industrial types of equipments. They have been found suitable
for application in steel mills and in glass rather than rubber plants8.
The Iraqi bentonite molecule is formed in general from 3 plates, 2 of which
silicon oxides penetrated with a third plate of aluminum oxides. Those plates are
surrounded with cloud of positive ions of calcium9.
The bentonite soils have the ability to swell when absorbing water. This abil-
ity increases when attraction forces for a single molecule decreases between the
molecule and the rest of surrounding molecules. Since Iraqi bentonite is a cal-
cium type, and calcium is very hard in water because it is consisted of 2 positive
charges that giving it a high attraction force in comparison with a single posi-
tive charged molecule. Organophilic bentonite was prepared from the reaction of
bentonite with a long alkyl chain quaternary ammonium salt. Greases were then
prepared by dispersing the organophilic bentonite into a lubricating oil and mill-
ing through a triple roll dispersion mill10].
295
 In this research water resistance grease was directly prepared by ion ex-
change operation of calcium element. Accordingly the general reaction express-
ing the ion exchange process is formed by the following equation:
  
∆
2[(C2 H5)4 NCl] + [bent.Ca+2] → bent. [(C2H5)4N] 2 + CaCl2
HO
   2
The aim of present research is to prepare water-resistant grease from certain
raw Iraqi bentonite that can withstand high temperature and to select the suitable
operating parameters to prepare the grease.

experimental

Materials & Method

1. Base oil: mineral stocks were supplied from Al-Dora refinery; the mineral oils
were of stock 60 and 150. Table 1 shows the technical specifications of the used
base oils.
2. Bentonite soil: was purchased from the State Company for Geological Sur-
vey and Exploration. Table 2 shows the metallic and chemical composition of
Iraqi soils used in preparing the grease in the present research.
3. Quaternary ammonium salt (tetraethyl ammonium chloride, and tetraethyl
ammonium bromide)11, the specifications of the used salt are: anhydrous, colour-
less, odourless, hydrogroscopic crystals, free soluble in water, alcohol, chloro-
form and acetone, slightly soluble in ether, and with purity of 98%, supplied from
Fluka.
4. The dispersion agent was methyl alcohol (Fluka), specific gravity (0.7910),
and flash point of 65˚F.

Table 1. Specifications of the used base oils

Specifications Stock 60 Stock 150

Viscosity (cSt)
at 40°C 60 – 90 460 minimum
at 100’C 8 – 10 30 – 35
V.I 95 minimum 93 minimum
Pour point (°C) –6 maximum –3 maximum
Colour* 1.5 3
Flash point (°C) 250 minimum 260 minimum

* The colour of oil is measured by a Lovibond apparatus, thus it is a comparison with standard
colours; it gives knowledge of products pollution and the difference of physical and chemical prop-
erties from international specifications.

296
Table 2. Chemical Composition and Mineralogy of Iraqi soil9

Metal (%) Range (%) Average (%)

chemical composition
SiO2 54.61  –  59.83 56.77
Al2O3 13.70  –  16.69 15.67
Fe2O3   4.88  –  5.66  5.12
CaO   2.80  –  5.80  4.48
MgO   3.06  –  3.76  3.42
Na2O   0.65  –  1.80  1.11
K 2O   0.40  –  0.90  0.60
P2O5   0.47  –  0.91  0.65
SO3   0.10  –  1.95  0.59
Cl   0.10  –  1.22  0.57
L.O.I   8.37  –  13.27  9.49
C (total carbon)   0.24  –  1.20  0.56
Impurities   0.95  –  1.00  0.97
Total 100%
Mineralogy
Montimorlonite 70 – 85 80
Palygorskite 5 – 10  7
Quartz and chalcedony 3–7  5
Calcite 1.6 – 5.59  4
Apatite 1.4 – 2.2.7  2
Gypsum 0.2 – 3.9  1
Halite 0.2 – 1.8  1
Total 100%

5. The medium for ion exchange was adequate and suitable volume of dis-
tilled water (200 ml for every 100 gm).

Equipments

Stainless steel autoclave with capacity of (0.5 l) – Parr Instruments Company

(USA), control motor – Bodine Elictric Company (Chicago, USA), oven with elec-
tric drying over (50–200°C) (Toyo Seisakusho, Nihonbashi, Japan) and Miller-
Karl-Kolb Scientific Technical Supplies (Germany).
The preparation of grease samples was carried out by 3 steps:

1. Ion exchange (treating of Iraqi bentonite). A pre-estimated proportion of qua-

ternary ammonium salt and bentonite were mixed in presence of suitable volume
of water (200 ml) as ion exchange medium at a temperature lower than the boiling
point; the chosen temperature was (75°C), accompanied with mixing for 30 min.
The flocculated clay (thickener) was dried in oven at 110°C, pulverised and milled
to 200 meshes (45 µm).
297
2. Mixing the grounded flocculated clay with oil. A mixture of base oil and metha-
nol (1% methanol from base oil) was prepared, then the treated bentonite was
added to the mixture with continuous stirring (500 rpm.) for 30 minutes. The
temperature was raised to 40°C followed with additional mixing for 30 min. to
sweep away air bubbles formed during the treatment.

3. Addition of additives. 7% wax was added to raise the solidity and adherence of
the prepared grease. Wax addition is respected to prevent isolation between the
oil and the thickener. Asphalt was added for some grease samples to increase the
viscosity of the grease for sealing purposes uses12.

Analysis Methods

Swelling measurement was done according to the procedure in Ref. 10. Viscosity
test for base oil was carried out by viscometer type Schott-Gerate-Gmbh (Germa-
ny). Penetration number for the prepared grease was carried out by a penetrotme-
ter surBerline, Ablesung 1/10 mm type (Germany). Dropping point was carried
out according to the procedure in Ref. 13 by the equipment type Analis Belgium
Company (USA). Water resistance was made at Al-Dora refinery lab according to
ASTM D-1264 (Ref. 4).

Results and discussion

The addition of 7% by weight wax was respected as the most appropriate to pre-
vent separation between oil and thickener in the prepared grease especially in
case of using a blend of base oil and in case of using slightly viscous base oil to
increase its viscosity.
Firstly treated bentonite was dispersed in base oil using high temperature
usually by raising it up to 120°C without addition of any dispersion agent8. This
method was unsuccessful due to: the non occurrence of the required homogene-
ity, the treated bentonite was accumulated in some regions, and isolation of the
base oil14.
Secondly, grease samples were prepared at a temperature not higher than
40°C with addition of 1% by weight methanol as suitable dispersion agent. Mix-
ing of the 2 stocks (60 and 150) for (30 min) was found to be necessary to ensure
a homogenous blend. Additional mixing of the methanol, thickener and oil blend
for 1 h accompanied with heating not higher than 40°C was needed to increase
the degree of dispersion and furthermore to sweep away the entrapped air. Tem-
perature higher than 40°C is not advisable due to the possible loss of dispersion
agent functioning. In this research the influencing factors are taken constant in
the preparation of grease except that for the concentration of reacting ingredients
which were optimised.
298
 Tables 3 and 4 show the NLGI (Na- Table 3: NLGI grade of prepared grease as
tional Lubricating Grease Institute) grade a function of different weight percentage of
treated bentonite with base oil 50% stock 60
number and the penetration point of the and 50% stock 150
prepared grease at different percentages
of the Iraqi bentonite, respectively: the Treated bentonite (% wt.) NLGI number
grease was prepared using blended oil 10 1
15 2
consisting of 50% stock 60 and 50% stock
20 2
150 with viscosity of 175 cSt at 40°C. 25 2
It was noticed that increasing the 30 2
percentage of added bentonite in the pre- 40 3

Table 4. Penetration point of prepared grease as a function of different weight percentage of treat-
ed bentonite with base oil 50% stock 60 and 50% stock 150

Treated bentonite (% wt.) Penetration point (mm)

10 313
15 294
20 286
25 277
30 269
40 248

pared grease leads to a decreasing in the penetration point which increasing the
consistency or stiffness of the grease. These results are in agreement with the
NLGI classification system15, and optimum penetration for bentone lubricating
greases14.
Grease samples were also prepared using stock 60 only. Results indicated that
increasing the amount of bentonite produced grease specimens having touch, no
odour, moderate consistency in-between liquidity and solidity with a pale brown
colour. The drop point of the prepared grease was also studied and the results are
listed in Table 5.
It was noticed that increasing the percentage of bentonite in the prepared
grease led to a corresponding increase in drop point and water resistance. Stock
150 was used alone in preparation of
Table 5. Drop point of prepared grease as
grease. Table 6 shows the grease wash function of different weight percentage of
out by tap and raw river water. It is seen treated bentonite with base oil 100% stock 60.
that by increasing the quantity of benton-
ite, the resistance to grease wash out by Treated bentonite (% wt.) Drop point (°C)
10 119
water was increased due to the increasing 15 124
in adherence force; the reason that the 20 130
percent of oil in the mixture decreases 25 137
and emulsified by water, then the result- 30 145
ing grease will be more massive. The ef- 40 163

299
Table 6. Water resistance of prepared grease as a function of different weight percentage of treated
bentonite with base oil 100% stock 1so
Washed out grease (g)
Treated bentonite (wt %)
tap water raw river water
10 5.2 7.5
15 4.1 6.1
20 3.3 5.5
25 2.7 4.3
30 2.1 3.9
40 1.0 2.5

fect of using river water on grease wash out is expected because of increase in salt
content which have a destructive effect on grease composition and, consequently,
on the efficiency of grease. Duplication of the experiments was done in order to
eliminate error encountered; the error between experiments was found to be in a
range of ±10%. A correlation was found describing the grease wash out; the cor-
rection coefficient of the two experiments was 0.9906 and 0.9970, respectively.
Stock 150 plus 5% asphalt (S-125 cut-back bitumen) was use in preparation of
grease with bentonite in ratio of 20 and 30% weight. Tables 7 and 8 show a com-
parison between NLGI number, penetration, drop points, and grease resistance to
wash out by water using 20 and 30% by weight of bentonite for grease prepared
from different base stock oils.
From Tables 7 and 8 it is noticed that by increasing the viscosity of the base
oil the resulted consistency was increased (decrease in penetration, drop points
and the resistance to water washout) at the same percent of added bentonite as
thickening agent.
Additionally, these results indicate that using 5% (by volume) asphalt with
95% stock 150 (causing an increase in the viscosity measured to be equal to 575
cSt) had raised the drop point and resistance to water washout considerably; con-
sequently a decrease in penetration point could be expected. It was also noticed
Table 7. NLGI number, penetration, drop point and grease resistance to water for grease prepared
from: 50% stock 60 and 50% stock 150, and only Stock 60
Type of base oil
50% stock 60 and 50% stock 150 stock 60
Viscosity (cSt)
Type of test
167 67
Percent of bentonite (wt.%)
20 30 20 30
NLGI number 2 2 1 2
Penetration point(mm) 286 269 311 290
Washed grease (g) (salt water) 6.4 5.2 7.9 6.3
Drop point (°C) 151 168 130 145

300
Table 8. NLGI number, penetration, drop point and grease resistance to water for grease prepared
from: only stock 150, and 95% stock 150 and 5% stock asphalt

Type of base oil

stock 150 95% stock 150 and 5% asphalt
Viscosity (cSt)
Type of test
414 575
Percent of bentonite (wt.%)
20 30 20 30
NLGI number 2 3 – –
Penetration point(mm) 253 240 311 290
Washed Grease (g) (Salt water) 5.5 3.9 4.5 2.6
Drop point (°C) 199 220 222 250

that the prepared grease had a smooth touch and almost rigid with approximately
black colour. The visual adherence of the grease was very high even in salty water
medium thus it could safely presume that successfully used as a sealant.

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Received 14 November 2012
Revised 2 January 2013
301

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