H.H. Abou El Naga,.

Production of a Transformer Oil from

A. Anis, A.E. Salem,
and Y.M. Boghdady Paraffinic Basestocks
Research Centre,
MlSR Petroleum Co.,

* Now with the Societe

Cooperative des Petroles,
Cairo, Egypt

Abstract The work described in this paper is concerned with the produc-
tion of a high quality transformer oil from local Egyptian par-
affinic basestocks. Analysis showed that a neutral base oil 70N
was most suitable for producing transformer oils. This neutral
base oil was chemically treated with a sulphonation process.
Optimum sulphonation conditions were achieved by using ole-
u m or SO3 at a concentration of 6 wt.%. The sulphonation reac-
tion was carried out in three stages, each with a n equal portion
of the sulphonating agent. The acidic oil was then neutralised
with a n alkaline solution. Oil colour improvement was effected
using activated clay as an absorbent. Laboratory results and
field trials indicated that such a treated neutral parafinic oil
meets the IEC 296 international specifications for transformer
oils, with the exception of pour point (-12 “c). However, such a
pour point is not relevant in certain hot climatic conditions.
Comparative evaluation of the treated oil with commercial
transformer oils has shown its suitability.

Keywords transformer oil, paraffinic, naphthenic, sulphonation, tests

INTRODUCTION The manufacture of a transformer oil begins with selection of

the proper type of crude oil - naphthenic, paraffinic or mixed
base.
Naphthenic crudes have been used for a long time, as
they contain a lower concentration of waxes and aromatics.
However, necessity has pushed some countries of the world to
use mixed-base or paraffinic crudes.’ All petroleum crudes can
be treated by suitable combination of processes to produce a
useable transformer oil; treatment processes are applied in
order to eliminate undesirable compounds while retaining
those that are desirable.2 Selection of such a combination of
treatment processes is not an easy task.

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
from Paraffinic Basestocks

Table 1 Properties of local (Egyptian) paraffinic neutral basestocks

Test Test Basestocks Limits of IEC

method 296
specification
70N lOON 140N 150N 250N

Kin. visc. Q 40°C, IP71 14.1 23.61 30 31.27 54 max. 16.5

mm2/s
Kin. visc. Q -15"C, not measurable max. 800
mm2/s
VI IP226 107 102 95 195 95 40-60
Flash point (PMCC),"C IP34 140 160 171 0.1 204 min. 140
Sulphur content, wt.% IP242 0.06 0.1 0.18 0.1 0.2 N.R.*
Foam:
Seq. 1 201zero 5QIzero 30/Zt?YO 301ZerO 3 0 1 2 ~ 0
Seq. 2 IP 146 201zero 1Qlzero 201zero 1Qlzero 1Olzero N.R.
Seq. 3 8Qlzero 3QIzero 50lzero 40/ZerO 5Qlzero
Induction time, min IP 229 30 17 15 36 16 -
Pour point, "C IP 15 -3 -5 -5 -5 -5 -30
Density Q 20"C, kglm3 IP 160 0.8612 0.8600 0.8660 0.8665 0.8790 max. 0.895
Breakdown voltage, kV IEC 10 11 8 3 10 min. 30
(as delivered) 156
Air release, minutes IP 313 1 3 5 3 4 N.R.
Molecular weight ASTM 352 360 390 400 420 N.R.
D-2502
Infrared spectroscopy Brand's
CA, mol.% method 12.26 10.13 13 9.53 12.8
Cp, mol.% 60.53 59.07 63 65.64 63 N.R.
CN,mol.% 27.21 30.80 24 24.83 24.2
Copper strip corrosion IP 154 1A 1A 1A 1A 1A N.R.
Ash, W.% IP 4 0.01 0.01 0.01 0.03 0.01 N.R.
Conradson carbon, IP 13 0.03 0.03 0.03 0.5 0.05 N.R.
wt.%
Colour ASTM 1 2.5 3.5 0.5 4.5 N.R.
D-1500
* N.R. = not recorded

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
from Paraffinic Basestocks

Several treatment techniques are used for producing

transformer oils. However, the first step is to obtain a suitable
distillate via the traditional refining steps, i.e. atmospheric
distillation, vacuum distillation, solvent extraction and dewax-
ing. The distillate obtained must then be treated with one or
more of the following processes: sulphonation, hydrotreating
a n d o r hydrogenation.
Some years ago, the acid treatment process was the only
accepted one, but in reality it was a dual process, as it was com-
bined with clay treatment.3 The other common processes are
hydrotreating or hydrogenation. These two processes are of dif-
ferent severity in the treatment of o i k 4 hydrogenation can dif-
fer from hydrotreating in terms of temperature and pressure,
but usually also employs a different c a t a l y s i ~ . ~
The objective of this work is to describe production of a
transformer oil from one or more local (Egyptian) paraffinic
basestocks via the sulphonation process. Selection of the
proper sulphonation conditions is the main consideration, and
these conditions must be selected to provide a transformer oil
in accordance with IEC 296 international specifications.

The properties of five local paraffinic basestocks were evalu-

ated to use in producing this transformer oil. The results of the
Basestock
analysis of these five basestocks are given in Table 1.
selection

Treatment The main process involves treating the selected basestock with
techniques a proper sulphonating agent under different sulphonation con-
ditions. Reaction variables depend on the degree of refinement
required for the selected basestock. The acidic oil is then neu-
tralised with an alkaline solution and, finally, the oil’s colour
improved with active clay.
In order to select the optimum sulphonation conditions,
several reaction tests are carried out, using one of the following
sulphonating agents: dry SO3 or oleum (concentrated sulphu-
ric acid). These reaction tests include different dosages of sul-
phonating agents, at different temperatures and for variable
times. Sulphonation reactions are carried out according to the
following steps:

(1) The selected basestock is first dewaxed according to a tra-

ditional procedure, e.g. dissolving the oil in a mixture of 1:l

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
from Paraffinic Basestocks

methyl ethyl ketone:toluene, then cooling this mixture to

-3O"C, and filtering it t o remove precipitated waxes.
(2) The dewaxed oil sample is brought t o a temperature suit-
able to start the sulphonation reaction. The following temper-
atures were investigated here as starting temperatures: 15,
25,35,45, and 55°C.
(3) The sulphonation agent (conc. H#04 (oleum) or SO3) is
added t o the oil in one or more stages. This addition is carried
out with continuous stirring at low speed (150 rpm). After each
addition of the sulphonation agent, stirring is continued for a
further 5 min. The percentage of each sulphonating agent add-
ed to the oil is changed as follows: 3 , 6 , 9 and 12 wt.%.
(4) After addition of each of the first two portions of the sul-
phonation agent, the acidic oil is allowed to settle (10-15 min)
to separate any excess sulphonation agent.
(5) After addition of the third portion, the acidic oil is allowed
to settle for about 4 h, in order to separate most of the remain-
ing sulphonation agent.
(6) The acidic oil is neutralised with an alkaline solution con-
taining 20 wt.% Na2C03.
(7) The neutralised oil is then washed with a suitable agent,
e.g. water or isopropyl alcohol, at a given temperature. Wash-
ing must continue until the oil is free of any salts.
(8) The treated oil is then analysed and, in the case of its
acceptability as a transformer oil, is kept in storage under an
N, blanket.

Analysis of untreated and treated basestocks is carried

out using IP test methods, as listed in Table 1.

RESULTS AND The following paraffinic basestocks have been considered, in

DISCUSSION: order to evaluate their suitability in producing a transformer
Basestock oil: 70N, 100N, 140N, 150N, and 250N, according t o the proper-
evaluation ties given in Table 1. Comparison of these results shows that
the oil most close to IEC 296 requirements is the neutral base
oil 70N. This oil has demonstrated the following properties:

(1) Kinematic viscosity at 40°C within the IEC 296 limits

(max. 16.5 cSt)
(2) Acceptable air-release and foam characteristics, which
show its low content of polar groups

~ ~~

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
from Paraffinic Basestocks

(3) A relatively good oxidation stability, with an induction

time (IP 229) of 30 min. This shows its naturally good
inhibition
(4) An acceptable sulphur content (0.06 wt.%)
(5) A relatively high naphthenic content (CN%27.21)
(6) An acceptable colour
(7) Within the IEC 296 limits concerning flash point, neutral-
isation number and density.

However, the candidate 70N basestock has a relatively

high viscosity index and pour point. The target of the treat-
ment processes is to help overcome such drawbacks, i.e. to get
the treated oil within the IEC 296 specification limits.

Addition time and The sulphonation parameters are chosen to remove some of the
acid dosage aromatics and sulphur content, but not all. According t o the lit-
erature,6-' it is essential to retain in the oil some aromatics
and sulphur content, as these compounds behave as natural
inhibitors, and improve oxidation stability, increase the oil's
capability to absorb evolved gases, and improve electrical prop-
erties.
To select the optimum addition time, i.e. the time neces-
sary for the addition of the sulphonation agent to the basestock
70N, trials were conducted under the following conditions.

(1) Addition of the sulphonation agent was varied over 30,60,

90 and 120 min.
(2) Oleum, as a sulphonating agent, was added in the follow-
ing percentages to the oil: 3,6, and 9 wt.%.
(3) The sulphonation reaction was performed at 35°C.
(4) The sulphonation agent was added in three stages, in
equal portions at each stage.

The following two parameters were considered in order to

evaluate the suitability of the addition time:

(1) Amount of unsulphonated oil produced (i.e. reaction yield

wt.%), to be as much as possible.
(2) The value of the breakdown voltage of the produced oil. It
is imperative that only oils with a breakdown voltage over 50
kV are acceptable. To rely on 30 kV, as mentioned in IEC 296,

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
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Figure 1 Change of reaction yield and breakdown voltage with addition time

Reaction 80 80
temperature 8 75 75

-
c
35°C
70 70 2
Y 3% oleum addition 65 65
o 6% oleum addition 5 6o 60
* 9% oleum addition “0
55
u
2c
55
50 50 5
2 45 45 5
2 40 40 m’
5
(0
35 35
30 30
30 60 90 120
Time. min

Table 2 Reaction yield and breakdown voltage for oil treated at 35°C with oleum

Acid dose, wt.%

3% oleum 6% oleum 9% oleum

Addition time, 30 60 90 120 30 60 90 120 30 60 90 120

min
Breakdown 33 40 42 44 34 56 57 57 35 55 56 56
voltage, kV
Unsulphonated 79 77 75.5 74 78 75.5 74 72.5 76 73 72 70.5
oil (yield),wt.%

is not acceptable, as treated oils are just produced and not yet
stored or shipped.

The results achieved with the candidate oil are given in

Table 2, and represented graphically in Figure 1.
The following conclusions can be drawn.

(1) An addition time of 30 min is relatively short for obtaining

an acceptable breakdown voltage, i.e. higher than 50 kV.
(2) With an addition time of 60 min or more, all the produced
oils are outside the breakdown voltage, i.e. higher than 50 kV.

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
from Paraffinic Basestocks

Figure 2 Change of re-

action yield and break-
down voltage with 3
reaction temperature 8 Yield Yo
$ 80 80
-0 '
s 2
I n "
._
(I) 0
Oleum 6 wt.% 4 60 Breakdown voltage, kV 60 2
Addition time 60 min -
.-
0 9
n
(I) 5-
5
0
40 140 0
B
r
-
Q ;
iC 2011 20
3

0 - 0

Table 3 Reaction yield and breakdown voltage for oil treated with oleum at different reaction
temperatures'

Reaction temperature, C O

15 25 35 45 55
Breakdown voltage, kV 19 22 56 46 40
Unsulphonated oil (yield), 86 79 75.5 74 71
wt.%
oleum 6 wt.%; addition time 60 min

(3) Extending the addition time for longer than 60 min did not
produce any remarkable improvement in the breakdown volt-
age of produced oils.
(4) None of the trials with 3 wt.% oleum gave oils with accept-
able breakdown voltage (i.e. lower than 50 kV).
(5) The highest reaction yield achieved was with 60 min addi-
tion time and with an oleum percentage of 6 wt.%; increasing
the oleum percentage to 9 wt.% produced a decrease in the re-
action yield, while the breakdown voltage remained approxi-
mately constant.

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
from Paraffinic Basestocks

As far as these results are concerned it can be concluded

that an acceptable balance between the wt.% yield and the
breakdown voltages can be achieved with an addition time of
60 min, and an oleum percentage of 6 wt.%.

The optimum sulphonation temperature was determined by

Effect of
varying the temperature of the sulphonation process, at 15,25,
sulphonation
35,45, and 55°C. Oleum was used as a sulphonating agent at
temperature
6 wt.%. The oleum addition time was kept at 60 min. Yield in
wt.% and breakdown voltages, at different reaction tempera-
tures, are listed in Table 3 and represented graphically in
Figure 2. The results give the following:

(1) The reaction temperatures of 15 and 25°C did not give

acceptable breakdown voltage values (i.e. gave all results low-
er than 50 kV).
(2) A reaction temperature at 35°C gives the highest break-
down voltage values.
(3) Any reaction temperature higher than 35°C (i.e. at 45 and
55°C) gives unacceptable breakdown voltage values (i.e. values
lower than 50 kV).

Accordingly, these results show that the optimum

sulphonation temperature is at around 35°C.

Effect of Dry SO3 gas Table 4 gives the results of using dry SO3 gas
sulphonating agent as a sulphonating agent, instead of oleum. SO3 gas was added
to the 70N basestock in the following dosages: 3, 6, 9, and 12
wt.%. From these results, it is clear that the balance in terms
of optimum breakdown voltage and wt.% yield can be achieved
by using SO3 gas at 6 wt.% in the base oil.
As expected, increasing the dosage of SO3 gas to more
than 6 wt.% can result in decreasing the percentage yield.

Concentrated H2S04 Table 5 includes the results of using

concentrated H2S04,as a sulphonating agent, at dosages of 3,
6, 9, and 12 wt.%. From these results, it is clear that concen-
trated (96-98%) H2S04 is very poor in terms of producing oils
with an acceptable breakdown voltage (i.e. with values higher
than 50 kV).All the oils produced showed a breakdown voltage
of less than 50 kV, decreasing as the acid dose decreases.

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
from Paraffinic Basestocks

Table 4 Reaction yield and breakdown voltage for oil treated using dry S q gas as a
sulphonation a g e d

Acid dose, wt. %

3 6 9 12

Breakdown voltage, kV 34 25 49 45
Unsulphonated oil (yield), 76 74 70 66
wt .OQ/
reaction temperature 35°C; addition time 60 min

Table 5 Reaction yield and breakdown voltage for oil treated by using conc. %SO4 as
sulphonating a g e d

Acid dose. wt. %

3 6 9 72
Breakdown voltage, kV 30 35 39 38
Unsulphonated oil (yield), 80 74 72 70
wt.%
* reaction temperature 35°C; addition time 60 min

Comparative Oleum us. SO3 gas Table 6 (see overleaf) gives the physico-
evaluation chemical and electrical properties for treated 70N basestock
after separate sulphonation with 6 wt.% each of oleum and dry
SO3 gas. Reaction temperature and addition time were 35"C,
and 60 min, respectively. An Na2C03 solution at 20 wt.% con-
centration was used as a neutralising agent, and active clay
was used as a bleaching agent.
Comparing the results with the IEC 296 international
specifications, it can be seen that:

(1) Both oleum and SO3 gas give transformer oils that possess
properties within the IEC 296 limits, in terms of the following:
a kinematic viscosity at 40°C lower than 16.5 cSt
a flash point (PM) greater than 140°C
a density at 20°C lower than 0.895 kg/m3
a neutralisation number lower than 0.03 mg KOWg
sample

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
from Paraffinic Basestocks

Table 6 Physico-chemical and electrical properties of treated neutral base oil 70N using
optimum acid dosage at 35°C and for 60 minutes

Test Test method Sulphonating agent (6 wt. %) Limits of

IEC 296
Dry so3 Oleum

Kin. visc. @ 40°C, mrn2/s IP 71 12.7 12.8 max. 16.5

Flash point (PMCC), "C IP 34 144 143 min. 140

Neutralisation number, IP 139 0.01 9 0.01 a max. 0.03

mg KOH/g sample

Colour IP 196 <0.5 zero N.R.*

Density @ 20°C, kg/m3 IP 160 0.8625 0.8630 max. 0.895

Pour point, "C IP 15 -1 2 -1 2 -30

Infrared spectroscopy
CA,mol.% Brand's 12.25 13.443
Cp,mot.% method 60.54 69.431 N.R.
CN, mol.% 27.21 17.126
Total 100 100

Sulphur content, wt.% IP 242 0.09 0.09 N.R.

Breakdown voltage, kV
as delivered IEC 156 52 56 min. 30
heating @ 70°C for 30 min 56 58 min. 50
storage under N2 57 59 -

Tan 6 @ 90°C and 40-60 Hz ASTM D-924 0.0030 0.0035 max. 0.005

Oxidation test:
induction period, min IP 229 40 38 -
total acidity, mg KOH/g sample IP 307 0.025 0.029 max. 1.5
total oxidation product, wt.% 0.098 0.1 max. 1.0
* N.R. = not recorded

the results of the oxidation test (according to BS 148 and

IP 307).
(2) Pour point and kinematic viscosity at -15°C for the
oils produced are not within the IEC 296 specification
limits (-30°C and 800 cSt respectively). It was not possible to
measure the kinematic viscosity at -15°C for the oils produced

~~

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
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Table 7 Comparative evaluation of treated neutral base oil 70N with another transformer oil

Test Test method Locally Commercial Limits of IEC

produced transformer 296
transformer oil
oil + dry SO,

Appearance Clear, free from sediment and suspended

matter
Kin. visc. Q 40"C, mm2/s IP 71 12.7 13.15 max. 16.5
Flash point (PMCC), "C IP 34 144 150 min. 140
Colour IP 196 <0.5 0.5 N.R.'
Density Q 20"C, kg/m3 IP 160 0.8625 0.8879 max. 0.895
Sulphur content, wt.% IP 242 0.08 0.07 N.R.
Infrared spectroscopy
CA,mol.% Brand's 12.25 11.158
Cp, mol.% method 60.54 49.767 N.R.
CN, mol.% 27.21 39.075
Total 100 100
Pour point, "C IP 15 -1 2 <-30 -30
with 500 ppm additive -30
Breakdown voltage, kV
as delivered IEC 156 52 35 30
heating Q 70°C for 30 minutes 56 45 50
Tan 6 Q 90°C and 40-60 Hz ASTM D-924 0.003 0.0032 max. 0.005

Oxidation test:
induction period, min IP 229 40 38 -
total acidity, mg KOH/g sample IP 307 0.025 0.029 max. 1.5
total oxidation product, wt.% 0.098 0.1 max. 1.O
* N.R. = not recorded

as their pour points were -12°C. However, in local climatic con-

ditions, such a low pour point is not necessarily relevant.
Treatment with SO, gas has given an oil with a relatively
high naphthenic content (27.21 mol.%).

Locally produced us. imported oil The locally produced trans-

former oil can be compared with a commercial transformer oil,
and Table 7 gives the analysis for these two oils in comparison

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
from Paraffinic Basestocks

with the IEC 296 specification limits. These results show that
both oils are within IEC 296 specification limits for kinematic
viscosity at 40”C,flash point and density. The local base oil has
a lower density (i.e. greater paraffinic content), higher break-
down voltage (as received), and a longer induction period (i.e.
higher oxidation stability). The imported oil contains a higher
percentage of naphthenic content (CN),i.e. mostly naphthenic,
with a paraffinic base oil. Such a high naphthenic content ex-
plains its low pour point and viscosity index.

Sulphonated Trials are being run using the sulphonated residues as start-
residue ing materials to synthesise oil-soluble detergent additives.

CONCLUSION Analysis of light and medium local (Egyptian) paraffinic base-

stocks has shown that the base oil 70N is the most suitable one
to use in the production of a transformer oil.
Sulphonation of this neutral oil with either dry SO3 gas
or fuming sulphuric acid (oleum) at 6 wt.% was found to give
transformer oils with breakdown voltages higher than 50 kV.
The reaction yield is quite acceptable at around 75 wt.%.
The sulphonation must be performed in three stages,
each using an equal portion of the sulphonating agent, and
taking a time of 20-30 min with slow stirring. The correct tem-
perature to start the sulphonation is 35°C. Careful separation
of the extra sulphonating agents must be carried out after each
stage. Oil neutralisation can be performed with 20 wt.% alka-
line Na2C03 solution.
A comparative evaluation of the oil produced with
another commercial transformer oil has shown its good
properties.
1. Renguet, J., ‘The refining and production techniques of transformer oils’,
References paper presented at the 5th International Seminar on Oils, Fuels and Additives,
Cairo, 1990.
2. Jansson, L.I., ‘Production techniques and optimisation of transformer oils
regardingelectrical parameters’, paper presentedat the 5th InternationalSeminar,
op. cit.
3. The Petroleum Hand Book, Royal Dutch/ShellGroup of Companies, London,
Sixth Edition, 1983.
4. Neumann, J., Lahme, P., and Severin, D., Composition and Properties of
Petroleum, Halsted Press, New York, 1981.
5. Abou El Naga, H.H., and Abdel Ghany, M.A., ‘Chemical structure base for
oxidation stability of neutral base oils’, ASLE Trans., 30 (1987).
6. Sreenivasan, C.S., and Krishnaswamy, K.R., ‘Development of high quality
transformer oil’, paper presentedat the 3rd LAWPSP Symposium, Bombay, 1982.

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H.H. Abou El Naga, A. Anis, A.E. Salem, and Y.M. Boghdady: Production of a Transformer Oil
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7. Wilson, A.C.M., Insulating Liquids: Their Uses,Manufacture and Properties,

Institutionof Electrical Engineers, London, 1980.
8. Peries, J.P., Ballon, A,, Letourneur, P., and Rossarie, J., ‘IFP-Total
hydrotreating processes for producing special oils, white oils and waxes’, paper
presented at the 8th International Seminar, ‘New Developments in Engine and
Industrial Oils, Fuels and Additives’, Cairo, February 1992.

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