ALKALINE EARTH METAL HYDROCARBYL PHENATES, THEIR SULPHURISED DERIVATIVES, THEIR PRODUCTION AND USE THEREOF

PHENATES D'UN METAL ALCALINO-TERREUX, LEURS DERIVES SULFURES, LEUR PRODUCTION ET LEUR UTILISATION

English Abstract

22935-934
ABSTRACT OF THE DISCLOSURE
An additive concentrate suitable for incorporation
into a finished lubricating oil composition, the additive concen-
trate comprising:
(a) a lubricating oil,
(b) a lubricating oil soluble sulphurised or non-
sulphurised alkaline earth metal hydrocarbyl phenate modified by
incorporation of from greater than 2 to less than 40% by weight
based on the weight of the concentrate of either (i) at least one
carboxylic acid having the formula:-
<IMG> (I)
wherein R is a C10 to C24 alkyl ox alkenyl group and R1 is either
hydrogen, a C1 to C4 alkyl group or a -CH2-COOH group, or an an-
hydride, acid chloride or ester thereof or (ii) a di- or polycar-
boxylic acid containing from 36 to 100 carbon atoms or an anhydride,
acid chloride or ester thereof, the concentrate having a TBN
greater than 300.

Claims

- 25 - 22935-934
THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. An additive concentrate suitable for incorporation
into a finished lubricating oil composition, the additive concen-
trate comprising:
(a) a lubricating oil,
(b) a lubricating oil soluble sulphurised or non-
sulphurised alkaline earth metal hydrocarbyl phenate modified by
incorporation of from greater than 2 to less than 40% by weight
based on the weight of the concentrate of either (i) at least one
carboxylic acid having the formula:-
<IMG>
(I)
wherein R is a C10 to C24 alkyl or alkenyl group and R1 is either
hydrogen, a C1 to C4 alkyl group or a -CH2-COOH group, or an
anhydride, acid chloride or ester thereof or (ii) a di- or poly-
carboxylic acid containing from 36 to 100 carbon atoms or an
anhydride, acid chloride or ester thereof, the concentrate having
a TBN greater than 300.
2. An additive concentrate according to claim 1 wherein
the lubricating oil comprises from 10 to 90% by weight of the
concentrate.
3. An additive concentrate according to either claim 1
or claim 2 wherein the alkaline earth metal of the lubricating oil
soluble alkaline earth metal hydrocarbyl phenate is either calcium,
magnesium or barium.

- 26 - 22935-934
4. An additive concentrate according to claim 3 wherein
the alkaline earth metal is calcium.
5. An additive concentrate according to any one of claims
1, 2 and 4 wherein the alkaline earth metal hydrocarbyl phenate
is a sulphurised alkaline earth metal hydrocarbyl phenate.
6. An additive concentrate according to any one of
claims 1, 2 and 4 wherein the hydrocarbyl phenate moiety of the
oil soluble alkaline earth metal hydrocarbyl phenate is derived
from at least one alkyl phenol, the alkyl group or groups of the
alkyl phenol or phenols containing from 9 to 28 carbon atoms.
7. An additive concentrate according to claim 5 wherein
the hydrocarbyl phenate moiety is derived from a C12-alkyl phenol
obtained by alkylating phenol with propylene tetramer.
8. An additive concentrate according to any one of
claims 1, 2, 4 and 7 wherein there is incorporated at least one
carboxylic acid having the formula (I) wherein R is an unbranehed
alkyl or alkenyl group.
9. An additive concentrate according to claim 8 wherein
in the carboxylic acid of formula (I) R is a C10 to C24 straight
chain alkyl group and R1 is hydrogen.
10. An additive concentrate according to any one of
claims 1, 2, 4, 7 and 9 wherein there is incorporated a mixture
of carboxylic acids of formula (I), which mixture is a commercial

- 27 - 22935-934
grade containing a range of acids, including both saturated and
unsaturated acids.
11. An additive concentrate according to any one of
claims 1, 2, 4, 7 and 9 wherein there is incorporated stearic acid.
12. An additive concentrate according to any one of
claims 1, 2, 4, 7 and 9 wherein there is incorporated a di- or
polycarboxylic acid containing from 36 to 100 carbon atoms or an
anhydride thereof.
13. An additive concentrate according to claim 12 wherein
there is incorporated either a polyisobutene succinic acid or a
polyisobutene succinic anhydride.
14. An additive concentrate according to any one of
claims 1, 2, 4, 7, 9 and 13 wherein there is incorporated either
component (b) (i) or component (b) (ii) in an amount from greater
than 10 to 35% by weight based on the weight of the concentrate.
15. An additive concentrate according to claim 14 wherein
components (b) (i) or (b) (ii) are incorporated in an amount in
the range from 12 to 20% by weight based on the weight of the
concentrate.
16. An additive concentrate according to any one of
claims 1, 2, 4, 7, 9, 13 and 15 wherein the TBN of the concentrate
is greater than 350.

22935-934
17. An additive concentrate according to claim 16 wherein
the TBN of the concentrate is greater than 400.
18. An additive concentrate according to any one of claims
1, 2, 4, 7, 9, 13, 15 and 17 having a viscosity at 100°C of less
than 1000 cSt.
19. An additive concentrate according to claim 18 wherein
the viscosity at 100°C is less than 500 cSt.
20. An additive concentrate suitable for incorporation into
a finished lubricating oil which concentrate is obtainable by
reacting at elevated temperature (A) either (i) a hydrocarbyl
phenol or (ii) a hydrocarbyl phenol and sulphur, (B) an alkaline
earth metal base added in either a single addition or in a
plurality of additions at intermediate points during the reaction,
(C) either a polyhydric alcohol having from 2 to 4 carbon atoms,
a di- or tri-(C2 to C4) glycol, an alkylene glycol alkyl ether or
a polyalkylene glycol alkyl ether, (D) a lubricating oil,
(E) carbon dioxide added subsequent to the, or each, addition of
component (B), and (F) sufficient to provide from greater than 2
to less than 40% by weight based on the weight of the concentrate
of either (i) a carboxylic acid having the formula (I) as defined
in claim 1 or an acid anhydride, acid chloride or ester thereof or
(ii) a di- or polycarboxylic acid containing from 36 to 100
carbon atoms or an acid anhydride, acid chloride or ester thereof,
the weight ratio of components (A) to (F) being such as to produce
a concentrate having a TBN greater than 300.
28

- 29 - 22935-934
21. A process for the production of the additive concen-
trate as claimed in any one of claims 1, 2, 4, 7, 9, 13, 15, 17
and 19 which process comprises reacting at elevated temperature
(A) either (i) a hydrocarbyl phenol or (ii) a hydrocarbyl phenol
and sulphur, (B) an alkaline earth metal base added in either a
single addition or in a plurality of additions at intermediate
points during the reaction, (C) either a polyhydric alcohol having
from 2 to 4 carbon atoms, a di- or tri- (C2 to C4) glycol, an
alkylene glycol alkyl ether or a polyalkylene glycol alkyl ether,
(D) a lubricating oil, (E) carbon dioxide added subsequent to the,
or each, addition of component (B), and (F) sufficient to provide
from greater than 2 to less than 40% by weight based on the
weight of the concentrate of either (i) a carboxylic acid having
the formula (I) or an acid anhydride, acid chloride or ester
thereof or (ii) a di- or polycarboxylic acid containing from 36
to 100 carbon atoms or an acid anhydride, acid chloride or ester
thereof, the weight ratios of components (A) to (F) being such
as to produce a concentrate having a TBN greater than 300.
22. A process according to claim 21 wherein component
(B) is lime.
23. A process according to either claim 21 or claim 22
wherein the weight ratio of component (B) to component (A) is in
the range from 0.4 to 10.
24. A process according to claim 21 wherein component (C)
is ethylene glycol.

22935-93
25. A process according to claim 21 wherein component (C) is
methyl digol.
26. A process according to claim 22 or 24 wherein component
(C) is methyl digol.
27. A process according to claim 21 wherein the carbon
dioxide (component E) is added subsequent to each of two or more
additions of component (B).
28. A process according to claim 22 or 24 wherein the carbon
dioxide (component E) is added subsequent to each of two or more
additions of component (B).
29. A process according to claim 21 wherein a diluent is
present.
30. A process according to claim 22 or 24 wherein a diluent
is present.
31. A process according to claim 21 wherein the reaction is
carried out in the presence of a catalyst.
32. A process according to claim 22 or 24 wherein the
reaction is carried out in the presence of a catalyst.
33. A process according to claim 31 or 32 wherein the

22935-934
catalyst is calcium chloride.
34. A finished lubricating oil composition which composition
comprises a lubricating oil and sufficient of the additive
concentrate as claimed in any one of claims 1, 2, 4, 7, 9, 13, 15,
17 and 19 to provide a TBN in the range from 0.5 to 120.
35. A finished lubricating oil composition according to
claim 34 wherein the lubricating oil is a marine lubricating oil
and sufficient of the additive concentrate is present to provide a
TBN in the range from 9 to 100.
36. A finished lubricating oil composition according to
claim 34 wherein the lubricating oil is an automobile engine
lubricating oil and sufficient of the additive concentrate is
present to provide a TBN in the range from 4 to 20.
31

Description

~3~ Case 6538(2~
ALKALINE EARTH METAL HYDROCARBYL PHENATES, THEIR SULPHURISED
The present invention relates in general to alkaline earth
mstal hydrocarbyl phenates and their sulphurised derivatives, their
production and use thereo~ a~ lubricating oil additive~. In
particular the present invention relates to concentrate additive
compositions comprising alkaline sarth metal hydrocarbyl phenate~
and their sulphurised darivativas having both a high total base
number (TBN) and an acceptable viscosity, to their production and to
their use as lubricating oil additives.
In the internal combustion engine, by-products ~rom the
combustion chamber often b1Ow by the piston and admix with the
lubricating oil. Many of these by-products form acidic matsrials
within the lubricating oil. This is particularly mArked in diesel
engines operating on low-grade fuels of high sulphur content wherein
corrosive acids are produced by combustion. The acids thereby
incorporated in the lubricating oil can include sulphur acid~
produced by oxidation oi sulphur, hydrohalic acids derived from
halogen lead scavengers in the fuel and nitrogen acids produced by
the oxidation of atmospherlc nitrogen within the combustion
chamber. Such acids cause deposition o~ sludge and corrosion of thP
baarings and engine parts leading to rapid wear and early breakdown
of the engine.
One class of compounds generally employed to neutralise the
acidic materials and disperse ~ludge within the lubricating oil are
the metal alkyl phenates and sulphurised metal alkyl phenates,
wherein the metal is an alkaline earth metal ~uch a~ calcium,
.

~s~
magnesium or barium. Both "normal" and "overba3ed" alkaline earth
metal alkyl phenates have been employed. The term "overbased" is
used to describe those alkaline aarth metal alkyl phenates in whLch
the ratio o~ tha number of equivalents o~ the alkaline earth metal
moiety to the number o~ equivalents of tha phenol moiety i9 graater
than one, and is usually greater than 1.2 and ma~ be as high as 4.5
or greater. In contrast, the aquivalent ratio oi alkaline earth
metal moiety to phenol moiety in "norntal" alkaline earth metal alkyl
phenates is one. Thus, the "overbased" material contains ~reater
than 20~ in excess o~ the alkaline earth metal present in the
corresponding "nonmal" material. For thi~ reason "overbased"
alkaline earth metal alkyl phenates have a grea~ar capability for
neutralising acidic matter than do the corresponding ~normal'~
alkaline earth metal alkyl phenate~.
lS The prior art teachas many methods for preparing both "normal"
and "overbased" metal alkyl phenates. One ~uch method for preparing
"overbased" alkyl phenates generally referred to as the "3ingla lime
addition" process comprises reacting an alkyl phenol, in the
prasence or ab~ence o~ sulphur, lubricating oil, a hydroxylic
compound and excess alkaline earth metal hydroxide (above the
~toichiometric proportion required to neutralise the alkyl phenol),
to form an intermediate product, followed by carbonation, a heading
distillation (to remove unreacted hydroxylic compound) and
filtration. The produc~ of intermediate product i9 accompanied
by a marked increase in viscosity while the subsequent carbonation
reduces the viscosity to a relatively low level. The increase in
viscosity acco~panying the formation of the intermediate product is
undesirable because the reaction mixture becomes dificult to
agitate to the detriment of subsequent reactions. Whilst this
increase in viscosity may be controlled to an acceptable level by
incorporation of less alkaline earth metal hydroxide in the
raaction, the overbased alkyl phenate product necessarily possesses
a reduced neutralisation capacity. In order to achieve a high
neutralisation capacity product and at the same time control the
viscosity of the inte~tediate product within acceptable limits, the

~3C~
slkalin~ earth metal hydroxld~ may be added in twol (gcnerally
referred to aq the "double lime addition" process) or three 3eparate
reaction step~, with ~qu~ntial carbonation 9tCp9. However, this
m0thod involves relatively long batch times. Another alt~r~ativa i9
to u~e vi~cosity depr~ant~, ~uch a3 trid~canol, 2-athylhexanol, or
3imilar boiling range hydroxylic aolvent, in the production of th~
intermadiate product but ~uch an expedient increase~ the raw
~aterial cost of th~ proces~. The highsst total base number (TBN),
e~pre~ed in mB KOH/g, con~istent with an acceptable vi~c09ity,
generally achiavabla by prior art proces3es i3 about 300, though
generally prior art TBN~ ars in the range from 200-300. It would
clearly be a desirabl~ ob~ective to produce an additiv~ concentrate
compri3ing alkaline earth metal alkyl phe~ates or ~ulphuri~ed
derivative~ ther~of having a hi8h TBN, that i8 a TBN 8reatQr than
300, ant pr0ferably greater than 350. To dat0 it has not been found
po3~ible to achieva products of ~uGh high TBN becau~e tha u~a of
larger concentrations o~ alkalin~ earth metal ba~e laads to highly
vi~cous product~ which, rathar than being 'thinned' by sub~nqusnt
carbonation attempt~ u~ing exces~ carbon dioxide, are rendered
inqoluble. We have ach~eved thi3 objectiv0 and thereby obtained
products having a TBN in excess of 300, and in ~ome cases 8reater
than 350, whilst retaining an acceptable visc03ity, that i~ a
vi~cosity at 100C of les3 than 1,000 cSt and avoiding insolubility
by incorporating into the re2ction mixtur0 a defined amount of
certain carb~xylic scids having at laast 10 carbon atom3 in th0
molecule or acid derivatives.
The u~e o~ carboxylic acid~ either in ~he production of
alkaline earth metal alkyl phenates and th~ir sulphurised
derivatives or in as~ociatlon therewith in lubricating oil
c~mpo3itions i3 not new, see for exampl0 US-A-3,372,116;
GB-A-1440261; US-A-4049560 and EP-A-0094814.
~S-A-3,372,116 disclo~e~ an improvement in tha method for
preparing a basic matal phanate by r0acting at a temperature between
about 25C and tha reflux temperature (A) a hydrocarbon-~ubstituted
phenol havine at least 6 casbon atom~ i~ the h~drocarbon

~3~S~
substituent, a mixture of 3aid phenol with up to an equivalent
amount of a hydrocarbon-substituted ~uccinic acid or anhydrida
having at least about 6 carbon atoms in th~ hydrocarbon substtuant,
or a substantially neutral alkali metal or &lkaline earth metal salt
or either of the foregoing, (B) about 1-10 eq~ivalents, per
equivalent of (A), of a calcium or strontium bas~, and (C) carbon
dioxide, which improvement comprises carrying out tho reaction in
the presence of about 0.002-0.2 aqulvalent, per equivalent of Yaid
calcium or strontium basa, o a carboxylic ecid having up to about
100 carbon atoms or an alkali metal, alkaline earth metal, zinc or
lead salt thereof. The preferred carboxylic acids are those
containing up to about 10 carbon atoms, more pr~ferred being
monocarboxylic acid~ containing up to 10 carbon atoms and alkaline
earth metal 3alts thereof. In many of the Examples water and a
carboxylate salt are employed. Not only do we wish to avoid the
presence of water but we also find that carbo~ylate salts can not be
used in the process o~ the present invention bacause of their
inherent insolubility in the system. The procoss of US-A-3,372,116
does not employ phenol to alkaline earth metal base ratios
sufficient to produce phenates having TBN~ in excess o~ 300.
GB-A-1440261 discloses a lubricating oil composition comprising
a lubricating oil, a detergent or di~persant additive and a mixture
of at least two carboxylic acids, one acid having a melting point of
at least 20C and not mo~ than 30 carbon atom~ per molecule, and
another acid having a melting point of balow 20C, the weight
proportion of low melting point acid to high melting point acid
being between 1.5:1 and 8:1. The detergent may be an overbased
phenate, those having a TBN of 50 to 100 being considered very
sultable. In the lubricating oil compo~ition the mixture of acids
30 i~ present in an amount of 0.05 to 2.0 wt ~.
US-A-4049560 describes the production of an overba~ed magnesium
detergent by a process in which carbon dioYide is introduced into a
reaction mixture which comprises:
(a) 15-40 wt % of a sulphurised phenol or thiophenol cont~ining one
or more hydrocarbyl sub~tituents, or a phenol or thiophenol

~3~
containing one or more hydrocarbyl substituents, or sald ph~nol
or thiophenol containing one or more hydrocasbyl substituents
together with sulphur,
(b) 5-15 wt ~ o~ an organic sulphonic acid, an organic sulphonate
or an organic 3ulphate,
~c) 5-15 wt % of a glycol, a C1 to Cs monohydric alkanol or C2 to
C4 alkoxy alkanol,
(d) 2-15 wt X of a magncsium hydroxide or active magne~ium oxid~,
(e) at least 0.l wt ~ o~ a Cl to Clg carboxylic acid, an anhydride
thereof, or an ammonium, an amine salt, a Group I metal or a
Group II metal salt of said Cl to Clg carboxylic acid, and
(~) at least 10Z by weight of a diluent oil tincluding any present
in components (a) and (b).
The amount of carboxylic acit (component (e)) 1s preferably in
the range 0.5 to Z.OS by weight. The product prepared by this
r~action is said to have a TBN of about 200 to 250, e.g. about 225.
EP-A-0094814 discloses an addit$ve roDcentrate for
incorporation in a lubrlcating oil co~position comprising
lubricating oil, and from 10 to 91) wt % o~ an overbased alkalina
earth metal hydrocarbyl sulphurisod phenate which has bean treated,
either during or subsequent to th6~ overbasing process, with from 0.1
to 10, prsferably 2 to 6, wt X (based on the weight of additive
concentrate) o~ an acid of the formula:
~ CH - COOH (I)
R
(wherein R is a Clo to C~4 unbranched alkyl or alkenyl group, and
i9 hydrog~n, a C1 to C4 alkyl group or a -CH2-COOH group) or an
anhydride or a ~alt thereof. Th~ ob;ect o~ the invention of
EP-A-0094814 is to overcome problems encountered with many additive
concentratss containing overbased additives, namely lack of
stability giving rise to sedimentation and foaming problems. The
problem o~ EP-A-0094814 is not ~hat of producing phenate additive
concentrates having a TBN of greater than 300 and indeed the
phenate additive concsntrates produced by the process of the

- 6 - 22935-934
invention, although demonstrating overcoming -the problems of
stability and ~oaming, have TBN values of less than 300.
It can be concluded that the prior art in which car-
boxylic acids are employed does not address the prob~em of
producing additive concentrates comprising overbased alkaline
earth metal hydrocarbyl phenates having a TBN of greater than 300
and an acceptable viscosity.
Accordingly, in one aspect the present invention
provides an additive concentrate suitable for incorporation into
a finished lubricating oil compositionr the additive concentrate
comprising
~a) a lubricating oil,
(b) a lubricating oil soluble sulphurised or non-
sulphurised alkaline earth metal hydrocarbyl phenate modified by
incorporation o~ from greater than 2 to less than 40% by weight
based on the weight of the concentrate of either (i) at least one
carboxylic acid having the formula:-
R - CH - COOH
Il (I)
wherein R is a C10 to C24 alkyl or alkenyl group and Rl is either
hydrogen, a Cl to C4 alkyl group or a -CH2-COOH group, or an
anhydride, acid chloride or ester thereof or (ii) a di- or poly-
carboxylic acid containing from 36 to 100 carbon atoms or an
anhydride r acid chloride or ester thereof/ the concentrate having
a TBN greater than 300.
Component (a) of the composition is a lubricating
.~
~ .

:~3~S~
- 6a - 22935-934
oil. The lubricating oil may suitably be ei-ther an animal oil,
a vegetable oil or a mineral oil. Suitably the lubricating oil
may be a petroleum-derived lubricating oil, such as a naphthenic
base, parafin base or mixed base oil. Solvent neutral oils are
particularly suitable. Alternatively, the lubricating oil may
be a synthetic lubricating oil. Suitable synthe-tic lubricating
oils include synthetic ester lubricating oils, which oils in-
clude diesters such as di-octyl adipate, di-octyl sebacate and
tridecyladipate, or polymeric hydrocarbon lubricating oils, ~or
~'

example liquid polyisobutenes and poly-alpha olefins. The
lubricating oil may suitably comprise from 10 to 90%, preferably
from 10 to 70%, by weight of thè composition.
Component (b) is a lubricating oil soluble sulphurised or
non-sulphurised, preferably sulphuri~ed, alkaline earth metal
hydrocarb~l phenate modified by incorporation of from greater than 2
to less than 40% by weight based on the weight of the composition of
either (i) or (ii). Suitably the alkaline earth metal may be
strontlum, calcium, magne3ium or barium, preferably calcium, barium
or magn2sium, more preferably calcium. The hydrocarbyl phenate
moiety of the alkaline earth metal hydrocarbgl phenate is preferably
derived from at least one alkyl phenol. The alkyl groups of the
alkyl phenol may be branched or unbranched. Suitable a~kyl groups
contain from 4 to 50, preferably from 9 to 28 carbon atoms. A
par~icularly suitable alkyl phenol i9 the C12-alkyl phenol obtained
by alkylating phenol with propylene tetramQr.
The alkaline earth metal hydrocarbyl phenate is modified by
incorporation of either (i) or (ii). As regards ~i), this is at
lea~t one carboxylic acld havlng the formula (I) or an acid
2G anhydride, acid chloride or ester thereof. Preerably R in the
formula (I) is an unbranched alkyl or alkenyl group. Preferred
acid~ of for~ula (I) are those wherein R is a Clo to C24, more
preerably Clg to C24 straight chain alkyl group and R1 is
hydrogen. Examples of s~table saturated carboxylic ac1ds of
formula (I) include capric acid, lauric acid, myri~tic acid,
palmitic acid, stearic acid, arachidic acid, behenic acid and
lignoceric acid. Examples of suitable unsaturated acids of
formula (I) include lauroleic acid, myristoleic acid, palmitoleic
acid, oleic acid, gadoleic acid, erucic acid, ricineleic acid,
linoleic acid and linolenic acid. ~ixtures of acid~ may also be
employed, for example rape top fatty acids. Particularly suitable
mixtures of acids are those co~mercial grades containing a range of
acids, including both saturated and unsaturated acids. Such
mixtures may be obtained synthetically or may be derived from

~5~i96
natural products, for exampla cotton oil, ground nut oil, coconut
oil, linseed oil, palm karnel oil, olive oil, corn oil, palm oll,
castor oil, soyabean oil, sunflo~ar oil, herring oil, sardinQ oil
and tallow. Sulphurised acids and acid mlxtures may also ba
amployed. Instead of, or in addition to, the carboxylic acid there
may be used the acid anhydride, the acid chloride or the ester
derivatives of the acid, preferably the acid anhydride. It is
preferred however to use a carboxylic acid or a mixture of
carboxylic acids. A preferred carboxylic acid of formula (I) is
stearic acid.
Instead of, or in addition to (i~, the alkaline earth metal
hydrocarbyl phenate may be modified by incorporation of (ii), which
is a di- or polycarboxylic acid containing from 36 to 100 carbon
atoms or an acid anhydride, acid chloride or ester derivative
thereof, preferably an acid anhydride thereof. Praferably (ii) is a
polyisobutene succinic acid or a polyi~obutene succinic anhydride.
Prefarably the carboxylic acid(s) having the formula (I), the
di- or polycarboxylic acid, or the acid anhydride, acid chloride or
ester thereof i~ incorporatHd in an amount from greater than lOX to
35%, more preferably from 12 to 20%, for example about 16Z by weight
based on the weight of the composition. An advantage of
incorporatine greater than 10% of the carboxylic acid or derivative
thereof is generally a relativelylower concentrate viscosity.
Suitably the alkal~`n~-e~rth metal may be present in th~
composition in an amount in the range from 10 to 20% by weight based
on the weight of the composition.
The alkaline earth metal hydrocarbyl phenate may be either
sulphurised or non-~ulphurised, preferably sulphurised.
Suitably sulphur may be present in the composition in an amount
in the range from 1 to 6, preferably from 1.5 to 3% by weight based
on the weight of the composition.
Suitably carbon dioxide may be present in the composition in an
amount in the ranga from 5 to 20, preferably from 9 to lS% by weight
based on the weight of the coMposition.
Preferably the TBN of the composition is greater than 350, more

~L3~,~6~6
preferably greater than 400.
Suitably the composition may have a viscosity measured at 100-C
o less than 1000 cStt preferably less than 750 cSt, more preferably
less than 500 cSt.
In another aspect the present invention provides an additive
concentrate suitable for incorporation into a finished lubricating
oll which concsntrate is obtainable by reacting at alevated
temperature (A) either ~i) a hydrocarbyl phenol or (ii) a
hydrocarbyl phenol and sulphur, (B) an alkaline earth metal base
added in either a single addition or in a plurality of additions at
intermediate points during th~ reaction, (C) either a polyhydric
alcohol having from 2 to 4 carbon atomsJ a di- or tri- (C2 to C4)
glycol, ~n alkylene ~lycol alkyl ether or a polyalkylene glycol
alkyl ether, (D) a lubricating oil, (E) carbon dioxide added
subsequent to the, or each, addition of component (B), and (F)
sufficient to provide from greater than 2 to less thaD 40% by weight
based on the weight of th0 concentrate of either (i) a carboxylic
acid having the formula (I) or an acid anhydride, acid chloride or
Qster thereof or (ii) a di- or polycarboxylic acid containing from
36 to 100 carbon atoms or an acid anhydride, acid chloride or ester
thereof, the weight ratio of components (A) to (F) being such as to
produce a concentrate having a TBN greater than 300.
In yet another aspect the present invention provides a process
for the production of an`~additive concentrate for incorporation into
a ginished lubricating oil which process comprises reacting at
elevated temperatura components (A~ to (F) as hereinbefore
described, the weight ratios of components (A) to (F) being such as
to produce a concentrate having a TBN greater than 300.
Component (A) of khe reaction mixture is either (i) a
hydrocarbyl phenol or (ii) a hydrocarbyl phenol and sulphur. Usi~g
component (A) (i) the product is an alkaline earth metal hydrocarbyl
phenate and u~ing component (A) (ii) the product is a ~ulphurised
alkaline earth metal hydrocarbyl phenate. The hydrocarbyl phenol
employed is that alkyl phenol from which is deri~ed the desired
hydrocarbyl phenate moiety as hereinbeiore described.

~31Q~6
lo
The alkaline earth metal base (component B) may suitably be an
alkaline earth metal oxide or hydroxide, preferably the hydroxide.
Calcium hydroxide may be added for example in the form of ~laked
lime. Preferred alkaline earth metals ara calcium, magnasiu~ and
barium and mora preferred is calcium. The alkaline earth metal base
must be added in an amount relative to component (A) suf~icient to
produce a product having a TBN in excess of 300, pre~erably in
excess of 3S0. This amount will depend on a number of iactors
including the natura oi the sulphurised alkyl phenol and will be
higher than the amounts generally employ~d in prior art processes.
Typically, the weight ratio o~ componsnt (B) to component (A) may
suitably be in the range from 0.2 to 50, preferably fro~ 0.4 to
10. The alkaline earth metal ba3e (~) may be added in whole to the
initial reactants, or in part to the initial reactants and the
remainder in one or more portions at a subsequent stage or stages in
the process. In order to produc~ an additive concentrate having a
TBN greater than about 350 and a viscosity at 100C of less than
1000 cSt it is particularly de~irable to add component (B) in at
least two, and preferably more additions and to add component (F) in
an amount greater than 10~ by weight based on the weight of the
additive concentrate product.
Component (C) i9 eithsr a polyhydric alcohol having from 2 to 4
carbon atoms, a di- or tri- (C2 to C4) glycol alkyl ether. The
polyhydric alcohol may s~itably be either a dihydric alcohol, for
example ethylene glycol or propylene glycol, or a trihydric alcohol,
for example glycerol. The di- or tri- (C2 to C4) glycol may
suitably be either diethylene glycol or triethylene glycol. The
alkylene glycol alkyl ether or polyalkylene glycol alkyl ether may
suitably be of ths ~ormula:-
R (ORl)XOR2 (II)
wherein R i~ a C1 to C6 alkyl group, Rl is an alkylene group, R2 i9
hydrogen or Cl to C6 alkyl and x i9 an integer in the range from 1
to 6. Suitable solvent~ having the ~ormula (II) include the
monomethyl or dimethyl ethers o~ ethylene glycol, diethylene glycol,
triethylena glycol or tetra~thylene glycol. A particularly suitable

~56~i
solv6llt is methyl digol (CH30CH2CH20CH2CH20H). Mixtures oi glycolsand glycol ethers of formula (II) may also be employed. Using a
glycol or glycol ether of fonmula (II) as solvent it is preferred to
use in combination therewith an inorganic halide, for example
ammoni~m chloride, and a lower, i.e. Cl to C~, carboxylic acid, for
example acetic acid. Preferably the component (C) i9 either
ethylene glycol or methyl digol, the latter in combination with
ammonium chloride and acatic acid.
Component (D) is a lubricating oil as hereinbe~ore described
with reference to the additive concentrate.
Component (E) is carbon dioxide, which may be added in the form
of a ~as or a solid, preferably in the form of a gas. In gaseous
form it may suitably be blown through the reaction mixture. We have
found that generally the amount of carbon dioxide incorporated
increases with increasing concentrations of component (F). In order
to produce a concentrate having a TBN greatsr than about 350 the
carbon dioxide is preferably added subsequent to each of two or
preferably more additions of component (B).
Component (F) is either a carboxylic acid of formula (I), a di-
or polycarboxylic acid containing from 36 to lO0 carbon atoms, or anacid anhydride, an acid chloride or ester thereof as hereinbefore
described with reference to the additive concentrate composition.
The amount of the aforesaid required to provide from greater than 2
to less than 40~ by weigh~ bassd on the weight of the concentrate
will be to a first approximation the amount desired in the
concentrate. In calculating th~s amount allowance should be made
for 103g of water from carboxylic acids, for example.
The reaction may be performed in the presence of a diluent.
Suitable diluents are liquids having a volatility consistent with
operation of the process, i.e. having a volatility such that they
are readily strippable from the reaction mixture at the conclusion
of the re~ction. Examples of suitable diluents include 2-ethyl
hexanol, iso-octanol, iso-heptanol and tri-decanol.
Preferably the reaction is carried out in the presence of a
further component which is a catalyst for the reaction. As catalyst
11

~L3a:~S~
there may ba used an inorganic halide which may suitably be eith0r a
hydrogen halide, an a~monium halide or a metal halide. Suitably the
metal moiety of the metal halide may be zinc, aluminium or an
alkaline earth metal, preierably calclum. Of the halides, the
chloride is preferred. Suitable catalysts include hydrogen
chloride, calcium chloride, ammonium chloride, aluminium chloride
and zinc chloride, preferably calcium chloride. Suitably the amount
of catalyst employed may be up to 2.0~ wt/wt.
Suitably the reaction of component~ (A) ~ (F) and also the
carbonation reaction may be carried out at elevated temperatures in
the range from 120 to 200, preferably from about 130 to 165C,
though the actual temperatures cho~en for the reaction of components
(A) - (F) and the carbonation may differ if desired. The pressure
may be atmospheric, subatmospheric or superatmo~pheric.
The concentrate may be recovered by conventional means, for
example by distillative stripping of component (C) and diluent (if
any).
Finally, it ic preferred to ~ilter the concentrate
so-obtained. Generally, ths process of the invention will produce a
concentrate having an acceptable viscosity, that is a viscosity of
less than 1000 cSt at 100~C, and can prod~ce concentrates having a
viscosity less than 750 or 500 cSt at 100C. Moreover, the
concentrates generally have desirable viscosity index properties.
Such viscometric propert`~es are advantageous because they facilitate
processing ~including filtration) of the concentrate. However, it
is also possibla to produce concentrates having a higher visco~ity
than 1000 cSt at lOO~C, generally at higher TBN levels. Filtration
of such concentrate~ presents a problem, which may be overcome by
adding a diluent prior to filtration and stripping the diluent off
after filtration. ~lternatiqely, high viscosity concentrates, for
example concentrates having a visco~ity at 100C greater than
1000 cSt, and also having a high TBN, ior example greater than 350,
may be diluted by addition of further lubricating oil whilst
maintaining a TBN greater than 300, thereby facilitating filtration.
In a final aspect the pre~ent invention provides a inished

:11 3~:~5~
lubricating oil composltion which composition compri3es a
lubricating oil and ~ufficient of the additive concentrate a~
hereinbefore described to provlde a TBN in the range from 0.5 to
120.
Preferably the finishet lubricating oil composition contains
sufficient of the additiva concentrate to provide a TBN in the range
from 0.5 to 100.
The amount of additiva concentrate presant in the fini~hed
lubricating oil will depend on the nature of the final use. Thus,
for marine lubricating oils the amount of additive concentrate
present may suitably be sufficient to provide a TBN in the range
from 9 to 100 and ~or automobile engine lubricating oils the amount
may suitably be sufficient to provids a TBN in the range ~rom 4 to
20.
The finished lubricating oil may also contain effective amounts
of one or more other types of conventional lubricating oil
additives, for exa~ple visco~ity index improvers, anti-wear agents,
antioxidants, di3parsants, rust inhibitors, pour-point depressants,
or the like, which may be incorporated into the finished lubricating
?.0 oil composition either directly or through the intermediacy of the
concentrata composition.
In addition to their use as additives for incorporation into
lubricating oil compo3itions, the additive concentrate of the
present invention may al~o find application as fuels additives.
The invention will now be ~urther illustrated by reference to
the following Example~.
In all the Examples the term "TBN~ is used. The TBN is the
Total Base Number in mg KOH/g as measured by the method o~
ASTM D2396.
The viscosity was measured by the method of ASTM D445.
In all the Examples, except otherwiqe expressly stated, a
comnercially available C12-alkyl phanol obtained by alkylating
phenol with propylene tetramer was employed.
Example 1
13

~3~5~
14
Char~: C12 alkyl phenol : 75 B
Lubricating oil (100 SN) : 131 g
Lime : 82 g
Sulphur : 23 g
Stearic acld : 70 g
Calcium chloride : 4 g
2-Ethyl hexanol : 112 B
Method
(a~ The charge was heated to 145-165C~700 mm Hg whilst adding
ethylene glycol (36 g),
(b) The m~xture wa~ heated at 165C/700 mm Hg for o~0 hour,
(c) Carbon dio~ida (40 g~ wa3 added at 165C/l bar,
(d) Tha mixture was cooled to 125C/700 mm H8,
(e) Lime ~35 g) was added at 125'C/700 ~m Hg,
15 (f) The mixture was heate~ at 165C/700 mm ~g ~or on0 hour,
(g) Carbon dioxide (20 g) wa~ added at 165C/l bar,
(h) The product was then ~tripped of solvent at 200C/10 mm Hg, and
(i) The product wa3 Pilterad. Ths filtration rats was fast.
Product Wei~ht
Crude Product : 436 8
Distillate : 169 g
P duct Composition After Filtration
Calcium : 14.1~ w/w
Sulphur ~ : 2.9~ w/w
25 C2 : 12.42 w/w
TBN : 396
VloO : 308 cSt
BPHV 150
Stearic acid : 16.1~ w~w
This Example demon~trate~ that a high TBN additivs concentrate
of acceptable vi~cosity can be produced in a "double lime addition"
proce~ acco-ding to the pre~nt invention.
Example 2
Charge: As for Example 1, except that the amount of lime in the
charge wa~ increased from 82 g to 117 g corresponding to
1~

::IL3~5~9~
tha total amount of lime added in Example 1 in two
additlons.
Method
As for Example 1 except that the amount of carbon dioxide added
in step (c) was increased from 40 g to 60 8 and ~teps (d), (e), (f)
and (g) were omitted. The filtrat~on rate in the final step was
slow.
Product Wei~ht
Crude Product : 514 g
Product Compo~ition After Filtration
Calcium : 14.1% w/w
Sulphur : 3.0% w/w
C2 : 12.3% w/w
TBN : 390
Vloo : 7600 c5t
Stearic acid : 13.6% w/w
This Ex~mple demonstrate3 that an additiva concentrate phenate
having a hlgh TBN can be produced in a singlQ lime addition process
but under the conditions of the Example the viscosity of the product
is unacceptable for commercial operation without dilution with
lubricating oil.
Example 3
Char~e: As ~or Example 1.
Method ~~
As for Example 1, except that in step (8~ the amount o~ carbon
dioxide was increased from 20 B to 40 g and the following steps wera
added after tep ~g) and before steps (h) and (i):
(j~ The mixture was cooled to 120C,
(k) Lime (35 g) was added at 120C,
(1) The mixture was heated at 165C/700 mm Hg, and
(m) Carbon dioxide (50 g) wa added to the mixture.
Product Wei~hts
Crude Product : 484 g
~istillate : 169 g

~3~
16
Product Composition After Filtration
Calcium : 15.8X w/w
Sulphur : 2.6~ w/w
C2 : 15.0% w/w
TBN : 439
Vl~o : 506 cSt
Stearic acid : 14.5~ w/w
This Example demonstrates that high TBN additive concentrates
can be produced by the process of the ~nvention by a tripla lime
addition.
Example 4
Charge: As for Example 1 except that the amount of lubricating oil
was r~duccd from 131 g to 158 g and the amount of stearic
acid was reducad from 70 B to 43 g.
Method
As for Example 1 except that in step (d) the mixture was cooled
to 135~C instead of 125C.
Product Wei~hts
Crude Product : 442 g
Distillate : 155 g
Product ComPOsition After Filtration
Calcium : 14.1% w/w
Sulphur : 2.9Z w/w
C2 ~-- : 11.9~ w/w
TBN : 393
V1OO : 3440 cSt
Stearic acid : 9.8Z w/w
This Example demonstrates by comparison with Example 1 that
although a high TBN product can be produced at an acid level less
than lOZ w/w the viscosity of tha product ls high.
E~ample 5
CharRe: C12-alkylphenol : 35.3 g
Lubricating oil (SN 100) : 131 g
Sulphur : 14.7 g
Calcium chloride : 4.0 g
1~

Stearic acid : 109.1 g
2-Ethyl hexanol : 224 g
Method
(a) The mixture was heated to 120C,
(b) Lime (82 B) was added at 120C/2~ Hg vacuum,
(c) Ethylene glycol (36 g) was added at 145 - 165C/2" Hg,
(d) The mixture was held at 165C/2" Hg for 1 hour,
(e) Carbon dioxide (40 g) was added,
(f) The mixture was c0012d to 130~C and lime ~35 g~ added at
130C/2" Hg,
(g) The mixture was held at 165C/2" Hg for 1 hour,
(h) Carbon dioxide (20 g) wa~ added at 165C,
(i) Solvent was stripped Erom the product at 200C/30" Hg, and
(;) The product was filtered.
~5~9s~ h~e
Crude Product : 397 g
Distillate : 245 g
Product Composition After Filtration
Calcium : 13.6% w/w
Sulphur : 1.2% w/w
C2 : 13.9~ w/w
TBN : 376
VloO : 142 cSt
V40 ~`- : 18~1 cSt
VI : 180
Carboxylic acid : 27.5% w/w
This Example demonstrates that a high TBN product having an
acceptable viscosity can be obtained using a stearic acid addition
oP 27.5% w~w based on the weight of the final product.
Example 6
CharRe: As for Example 5 except that the a~ount of C12-alkylphenol
was red~iced from 35.3 g to 15.fi g and the amount oP
stearic acid was increased from 10~.1 g to 128.7 g.
Method
As for Example 5.

S6~
1~
Product Weights
Crud0 Product : 416 g
Distillate : 242 g
Prcduct Composition After Filtration
Calciu~ : 14.5~ w/w
Sulphur : 1.0% w~w
C2 : 13.6~ w/w
TBN (mg KOH/g) : 395
V100 : 255 cSt
V40 : 3100 cSt
VI : 221
Stearic acid 5 30.9~ w/w
This F~xample demonstrates that a high TBN product can be
obtained at a stearic acid content of 30.9% w/w.
Examples 7 to 13
Char~e: As shown in the Table.
Method
(a) A mixture of alkyl phenol~ lubricating oll, calcium chloride,
stearic acid and 2-ethyl hexanol W~,3 heated to 120C/700 mm Hg,
(b) Lime was added at 120C/700 mm Hg,
(c) Ethylene glycol was added at 145 to 165~C/700 mm Hg and the
mixture was held at 165C/700 mm Hg for one hour,
(d) Carbon dioxide was added at 165C/l bar,
(e) Solvent was recovered at 200C/10 mm Hg, and
(f) The product was filtered.
Product Wel~hts
As shown in the Table.
Product Compositlon After Filtrati,on
As shown in the Table.
Th~ Examples demonstrate that an additive concentxate having a
TBN graater than 300 can be produced in a single lime addition'
process over a range of stearic acid contents rom 2.6 to 29.7% w/w
based on the weight of the concentrate.

TABL~
_ _ _ _ .
Exampls 7 8 9 10 11 12 13
_ . _ __
5 Stearic Acid
Content of Product 2.6 7.7 12.9 18.2 18.0 23.0 29.7
... . __ _ _ . ___
Char~e Wei~ht9 (R?
Lube oil 131 131 131 131131131 131
C12 Alkyl Phenol135 115 95 75 75 55 36
Lime 82 32 82 82 82 82 85
Sulphur 23 23 23 23 23 23 15
Stearic Acid 10 30 50 70 70 90 113
CaC12 4 4 4 4 4 4 4
2-EH 112 112 112 112112112 112
Ethylene Glycol 36 36 36 36 36 36 36
C2 28 28 28 28 40 40 40
_ _ _ _ _ _
Product wt (g) 389 391 386 385389391 382
Distillate wt (g)158 159 _ _ _ _
. . _ _ . _ . . _
Composition After
Filtration
Calcium (%) 11.2 11.011.1 11.211.011.111.1
Sulphur (~) 3.7 3.6 3.4 3.03.02.7 1.6
C2 (%) 6.5 6.9 7.1 6.58.210.810.2
TBN 314 310 311 310308312 302
Vloo (cSt) 286 190 163 160109128 84
_ __ _
Char~e: C12-alkyl phenol- : 64 g
Lubricating oil (SN 100) : 111 B
Sulphur : 20 g
Stearic acid : 59 g
Calcium chloride : 4 g
2-Ethyl hexanol : 190 g
Method
(a) The charge was heated to 120C/700 mm ~g,
(b~ Lims (70 g) was add~d,
(c) The mixture was heated from 145C to 165C/700 mm Hg whilst
addinB ethylene glycol (32 g),
19

S~ 6
(d) The mixture was held at 165C/700 mm Hg for 5 minutes,
~e) Carbon dioxide (44 8) was added at 165C/l bar,
(f) The mixture was cooled to 120C and l~me (oO g) was added,
(g) The mixture was held at 165GC/700 mm Hg for 5 mimltes,
(h) Carbon dioxide (44 g) was added at 165C/l bar,
(i) Solvent was recovered from the product by stripping at
200C/10 mm Hg, and
(;) The product was filtered.
Product We~hts
Crude Product : 408 g
Distillate : 245 g
Product ComPosition After Filtration
Calcium : 16.0~ w/w
Sulphur : 2.6% w/w
1s C2 : 14.6% w/w
TBN : 450
VloO : 488 cSt
Stearic acit : 14.5~ w/w
This Example demonstr~te~ that an additive concentrate havlng a
TBN as high as 450 and an acceptable viscosity can be produced by
the process of the invention.
Example 15
C12-alkyl phenol : 64 g
Lubricating oi~ (SN 100) : 111 g
Sulphur : 20 B
Stearic acid : 59 8
Acetic acid : 2 g
AMmonium chloride : 3 B
Methyl diglycol : 40 g
Method
(a) The charge was heated to 120lC/100 mm H~,
~b) Lime (70 g) was added,
(c) The mixture was haated from 145C to 165C~700 mm HB whilst
adding methyl diglycol (90 g),
(d) The mi~ture was held at 165~C/700 mm H8 for 1 hour,

6~6
(e) Carbon dioxide (34 g) was added,
(f) The mixture was cooled to 120C and lime (30 g) wa~ added,
(B) The mixture was held at 165C/700 mm Mg for 1 hour,
(h) Carbon dioxide (17 8) was added,
(i) Solvent was recovered by stripping at 200C/10 mm Hg, and
(;) The product was filtered.
Product Weights
Crude Product : 361 B
Distillata : 14S g
Product Composition A~ter Filtration
Calcium : 14.1Z w/w
Sulphur : 2.7~ w/w
C2 : 12 4% w/w
TBN : 394
VloO : 164 cSt
Stearic acid : 16.3% w/w
Thi~ Example demonstrates that methyl diglycol can be used as
component tC) and that ammonium chlorid~ can be used a~ the catalyst
in the procas~ of the invention.
Example 16
C4arge: C12-alkyl phenol : 64 g
Lubricating oil (SN 100) : 73 g
Clg-linear alpha-olefin : 38 g
Sulphur `~ : 23 g
Stearic acid : 59 g
Calcium chloride : 3 g
2-Ethyl hexanol : 190 g
Method
As for Example 15 except that in step (c~ instead of methyl
diglycol (90 g) there wa3 used ethylene glycol (31 g) and ln
~teps (d) and (B) th& mixture was hPld at 165C/700 mm Hg for
10 minutes instead of 1 hour
Product Wei~hts
Crude Product : 373 g
Distillate : 239 g

Product Composition After Flltration
Calcium : 14.4% w/w
Sulphur : 2.3% w/w
C2 : 13.3% w~w
TBN : 405
VloO : 460 cSt
Stearic acid : 15.8% w/w
This Example demonstrates that a long carbon-chain alpha-olefln
can be incorporated in the reaction.
Example 17
Char~e: As for Example 16 except that instead of the
Clg-alpha-olefin (38 g) there was used a polyisobutene
having an Nn f 500 (38 g).
Method
A3 for Example 16.
~c~
Crude Product : 363 B
Distillate : 246 8
Product Composition After Filtration
Calcium : 14.3% w/w
Sulphur : 2.8% w/w
C2 :13.8% w/w
TBN :406
V100 ` :697 cSt
V40 : 26,600 cSt
VI : 175
Stearic acid : 16.3% w/w
This Example demonstrates that a polyisobutene can be
incorporated in the reaction.
a8a:E~
Charg~: C12-alkyl phenol : 55.2
Lubricating oil (SN 100) : 131 e
Sulphur : 23 g
Calcium Chloride ' 4 B
Tallow Fatty Acid : 89.8 B
2-Ethyl hexanol : 112 g
22

~..3(~ 36
Method
As for Example 5 except that staps (f), (g) and (h) were
omitted, i.e. a single lime addition proce~s.
Product Wai~hts
Crude Product : 396 g
Distillate : 151 g
Product Composition After Filtration
Calcium :10.8~ w/w
Sulphur :3.1% w/w
C2 :11.3% w~w
TBN :305
Vloo :388 cSt
V40 : 20,000 cSt
VI : 101
Carboxylic acid : 22.7% w/w
This Exa~ple demonstrates that a high TBN addit~ve concentrate
can be obtained using a Tallow Fal:ty Acid.
Compari on Test
CharRe: C12-alkyl phanol : 75 g
Lubricating oil (SN 100) : 131 g
Sulphur : 23 g
Calcium chloride : 4 g
Acetic acid : 15 g
2-Ethyl hexano~ : 112 B
~ethod
As for Example 5 (a) - (d). Ther~a~ter tha mixture became a
thick heterogeneous mas~. Stirring wa~ ineEfectiv0 and the mixture
galled on cooling. The reaction ~as discontinued.
This Test demonstr~tes that acetic acid can not be used as the
carboxylic acid ln the process of the invention.
Example 19
Char~e: C12-alkyl phenol : 135 8
Lubricating oil (SN 100) : 131 g
Lime : 82 g
Sulphur : 23 g

~3~5~
Staaric acid : lO g
Calcium chlor$de : 4 g
Method
(a) The charge was heated to 145C/700 m~ Hg and iso-octanol
(112 g) was added,
(b) The mixtura was heated from 145C to 165Ct700 mm Hg and
ethylene glycol (36 g) wa~ added,
(c) The mixture was held at 165~C/700 m~ HB for 1 hour,
(d) Carbon dioxide (28 g) was added at 165~C/l bar,
(e) Solvent wa~ recovered by stripping at 210C/10 mm Hg, and
(f) The product was filtered.
Cruda Product : 380 g
Dl~tillate : 144 g
Product Composition After FiLtration
Calcium :10.8X w/w
Sulphur :3.6% w/w
C2 :6.0% w/w
TBN :301
VloO :216 cSt
Stearic acld :2.6X w/w