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l -‘ , do” designer I to
=
s
poem, Phiiadeip,
be" a corporation of Pennsylvc i
No
lr
i.
Application August 30, 19%, v
Serial No. 551,997
(Cl. 25%49-9)
i
a
The present invention relates to lubricant com
positions, and more particularly to rust-inhibit
ing lubricants suitable for the lubrication of
steam turbines, internal combustion engines,
gears, cables, and other metal surfaces exposed to
rusting or corroding conditions during use.
The lubricant of the present invention is es
pecially adapted for use in the lubrication of
' steam turbines, and has proved very satisfactory
mono- and diesters, or ixtures thereohmay be I
exempli?ed by the mono- and diphosphoridacld
esters of octyl alcohol, .nonyl alcohol, decyl al- .
cohol, undecyl alcohol, dodecyl alcohol, tridecyl ,
alcohol, tetradecyl alcohol,
pentadecyl alcohol,
_
and hexadecyl alcohol. The acid esters may be
simple mono- or diesters or mixtures of mono
and‘ diesters, and the alcohols employed in the
manufacture of the esters may besingle alcohols
in inhibiting rust and corrosion of turbine parts, 10 or mixtures of such-alcohols of from 8 to l?-car- '.
such rusting normally being caused by the steam
bon atoms, the alcohols having either s. straight
condensate entrained in the lubricants heretofore
chain or a. branched-chain structure.
,
employed.
'
The branched-chain alkylamines containing
The lubricant of the present invention is not
from 4 to 1!‘) carbon atomsjwhich may be used in,
only satisfactory from the view point of rust 15 the production-of the reaction product include
inhibition, but is likewise substantially una?ected
primary, secondary, and tertiary amines, or mix
by steam or water and retains a gooddemulsi
tures of two or more ‘ thereof.- Exemplary of
bility value during its use in steam turbines.
these compounds, all of which are characterized
'In accordance with the present invention, there
by the presence of branched-chain alkyl groups,
is added to a hydrocarbon oil, such as lubricating 20 are mono-, di-, and tri-isobutyl amines, tertiary _
oil of suitable viscosity, a small quantity of an
butyl amines, iso-amylamlnes, secondary amyl
oil-soluble reaction product of an alkyl acid phos
amines, tertiary amylamines, the branched-chain
phate having from 8 to 16 carbon atoms in the
hexylamines, heptylamlnes. octylamines, nonyl
alkyl group and a branched-‘chain alkylamine
amines, decylamines, undecylamines, dodecyl
containing from d to 16 carbon atoms in the 25 amines, tridecylamines, tetradecylandnes, penta
alkyl group. Such reaction product is preferably
decylamines, and hexadecylamines. In general.
pnepared by bringing equimolar quantities of
any alkylamine having a carbon chain of 4; to 10
thereactants to a temperature between 100° F.
carbon atoms and at least-one substituent alkyl
and 200° F. and e?ecting reaction between the
group of 1 to 4 carbons, constituting in into a
components at such temperature. It is believed,
branched-chain alkylamine, may be employed.
although not de?nitely known, that the reaction
In preparing the improved lubricant contain
produces anr addition salt since no byproducts
ing the rust-inhibiting reaction product, there‘ '
appear to be formed. The reaction. is usually
fairly rapid, with the evolution of heat, and the
reaction product usually comprises a clear, red
dish-brown, viscous oil. It is not necessary in
all cases to use exactly euuimolar proportions of
the acid phosphate and the amine, since it has
also may be added a small quantity ofv an anti- .
oxidant suitable for inhibiting the development
of acidity or of sludge in the oil. Various amines
or phenolic compounds may be employed. prefer
ably a naphthylamine such as phenyl alpha
naphthylamine, although other amines compati- '
been found desirable to have the reaction prod
ble with the rust inhibitor may be used.
uct slightly on the alkaline side, with a pH of 40
The quantity of'rust inhibiting reaction product '
about 8. This is accomplished by employing a
to be added to the lubricant ‘is usually small and
falls‘ within the range of 0.005% to 1%, the we
complete neutralization of the acid phosphate.
ferred amount being from 0.01% to 0.1% by
While it is preferred to cause direct reaction be
' weight. IThe antioxidant which may be utilized 0
tween the amine and the acid phosphate, such 45 in conjunction with the rust inhibitor has been > .
reaction may be carried out by adding the re
found satisfactory ‘in .amounts ranging ,from
actants to hydrocarbon oil, and then adjusting
slight excess of the amine over that required for .
the. temperature of the mixture to effect reaction,
' thus producing a hydrocarbon oil solution or the
0.05% to 0.55% by weight. 0.1% to 0.2% being ‘
preferred.
The present invention may be further illus- I
reaction product, which. if desired, may "be fur 50 trated
by the following example, which. however.
ther diluted with additional oil.
is not to be construed as limiting the scope
‘ The alkyl acid phosphates which may be uti
thereof.
‘
lined in making up the reaction product are the
A
mixture
of
monoand
dilauryl
acid
‘phos
mono- or dialwl acid phosphates having from 8
in which the monophosphate predoxnb
to 16 carbon atoms in the alkyl group.
a 55 phate,
noted, was placed in a reaction vessel and to '
i
2,418,852
effective for the designated
,
4 purpose, does not in
the mixture was added di-Z-ethyl hexylamine, the
temperature or the mixture being adjusted to
about 130° F. The mixture was thoroughly agi
tated and during the ensuing reaction, the tem
perature rose to aboutg200° F. The quantity of
amine added was su?icient to bring the pH of the
reaction product to about 8, and in the case of
these speci?c reactants, it was found that 1.1
parts by weight of the lauryl acid phosphate re
quired 1 part by weight of di-2-ethyl hexylamine
to produce the desired product of pH8, 'the amine
being present in slight excess of that required for
complete neutralization. The resulting reaction
product,_which appeared to be an addition salt,
consisted of a clear, reddish-brown, viscous oil.
crease the steam emulsion number or the neu
_ tralization number beyond permissible limits.
The lubricants of this invention,_while especially
adapted to the lubrication of steam turbines, are
alsosuitable for use in many other mechanisms
including internal combustion engines, compres
sors, gears, and the like.
. Ivclaim:
l. A lubricant comprising hydrocarbon oil and
a rust-inhibiting quantity of an oil-soluble re
action product 01 an alkyl acid phosphate having
from 8 to 16 carbon atoms in the alkyl group and
a branched-chain alkylamine containing from 4
to 16 carbon atoms in the alkyl group.
2. A lubricant comprising hydrocarbon oil, a
This material was added in various percentages,
rust-inhibiting quantity of an ‘oil-soluble re
with and without an antioxidant, i. e., phenyl
action product 01 an alkyl acid phosphate having ‘
alphanaphthylamine, to a selective solvent re
from 8'-to 16 carbon atoms in the alkyl group and
?ned lubricating oil having an A. P. I. gravityof
32° and a Saybolt universal viscosity of 155 sec-» 20 a branched-chain alkylamin'e containing i'rom 4
to 16 carbon atoms in the alkyl group, and air
onds at 100° F. The blank oil and the blends
amine antioxidant.
were then tested for rust inhibiting properties in
3. A lubricant comprising hydrocarbon oil and
accordance with ‘the A. S. T. M. Method D
i from 0.005% to 1.0% by weight or an oil-soluble
665-42T entitled “Method of Test for Rust Pre
venting Characteristics of Steam Turbine Oils in 25 reaction product of an alkyl acid phosphate hav
ing from 8 to 16 carbon atoms in the alkyl group
the Presence of Water.” Such test comprised
and ‘a branched-chain alkylamine containing
essentially immersing a polished steel strip in a
from 4 to 16 carbon atoms in the alkyl- group.
beaker containing 300 cc. of oil to be tested, rais
4., A lubricant comprising hydrocarbon .oil,
ing the temperature of the oil to 140° F. and stir
ring for 1/2 hour, removing 50 cc. of the oil and .50 from 0.005% to 1.0% by weight of an oil-soluble
reaction product of an alkyl acid phosphate hav
replacing with 30 cc. of water, continuing the
stirring at 140° F. for 48 ‘hours, removing the - . ing from 8 to 16 carbon atoms in the alkyl group
and a branched-chain alkylamine containing
steel strip and washing it with naphtha to re
1mm 4 to 16 carbon atoms in the‘ alkyl group,
move oil, and examining the strip for the percent
and from 0.05% to 0.5% by weight of an amine
surface rusted.
'
'
The results of the tests with the various oil
compositions are given in the following table.
antioxidant.
'
5. A lubricant comprising hydrocarbon oil and
a rust-inhibiting quantity of an oil-soluble reac- -
tion product of lauryl acid phosphate and (11-2
Condition of steel
strip
Oil composition
40
6. A lubricant comprising hydrocarbon oil, a
rust-inhibiting quantity or an oil-soluble reaction
Percent
rust in
1 hour
Blank oil"... _______________________________ ..
Blank oil+0.25% reaction product l...
. .
Blank oi_l+0.05% reaction product... .
Blank o1i+0.0l% reaction product
Blank oil+0.0l% reaction product-H) % anti
.
oxidant 3 .................................. _.
product of lauryl acid phosphate and di-2-ethyl
45
80
0
0
GO QO
! Luuryl acid phosphate-di-2’ethyl hexylamine.
'
ethyl hexylamine.
'-’ Phcnyl alpha naphthylamine.
hexylamine, and an oxidation-inhibiting quantity
of a naphthylamine.
7. A lubricant comprising hydrocarbon oil,
from 0.005% to 1.0% by weight of an oil-soluble
reaction product oi.’ lauryl acid,phosphate and
di-2-ethyl hexylamine, and irom 0.05% to 0.5%
by weight of phenyl alpha naphthylamine.
8. A lubricant comprising hydrocarbon oil,
about 0.01% by weight of an oil soluble reaction
As will be seen from the above data, the re
product of lauryl acid phosphate and di-2-ethyl
action product is compatible with the oxidation
hexylamine, and about 0.1% by weight of phenyl
inhibitor, and its rust inhibiting qualities are not
.
destroyed by the washing action of water. Fur 55 alpha naphthylamine.
thermore the presence of the inhibitor, with or
without the antioxidant, in the concentrations
"11R. TURNER.
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