Patented May 18, 1943

2,319,405
UNITED STATES PATENT OFFICE 2,319,405
MANUFACTURE OF GREASEs
Martin Hill Ittner, Jersey City, N.J., assignor to
Colgate-Palmolive-Peet Company, Jersey City,
N.J., a corporation of Delaware
No Drawing. Application August 3, 1940,
Serial No. 351,117
10 Claims. (C. 252-39)
This invention relates to novel greases that and claimed in my United States Patent No.
have a wide variety of uses and more particularly 1918,603 issued July 18, 1933, and United States
to lubricating greases, and methods for their Patent No. 1951,511 issued March 20, 1934, where
manufacture. in one or more of a great variety of different
Lubricating greases as ordinarily made con kinds of soap (water-soluble or insoluble) are
tain water or glycerine and usually both of these treated to remove volatile impurities including.
materials, which, in many cases, are highly ob glycerine with the aid of heat, usually with steam ...
jectionable in a grease. Both of these constit
uents might be looked upon with reason as ob
agitation and with substantial exclusion of air
or other oxidizing, influence.
jectionable impurities. Either or both of them () The Soaps are completely saponified and sub
may cause complete breakdown of a lubricating stantially pure. Where glycerine is formed in ,
film in a grease with the tendency for bad effects these Soap-making processes it is substantially
becoming more severe with increase in tempera completely removed and recovered, and the soap
ture or load. Both Water and glycerine act as produced is anhydrous and free from liquid water
solvents for one part of the grease and not for the or Water-containing emulsions unless water may
remaining part, and they lower the melting point . be subsequently added. The anhydrous soaps
of the grease and aggravate separation of the described in my two patents referred to above and
grease constituents. In those exceptional cases incorporated in my novel lubricating greases are
where glycerine may not be objectionable or may, characterized by an unusually low glycerine con
under unusual circumstances, be desirable, a very tent or none at all, freedom from volatile im
careful control of the quantity thereof is not only purities, and by a reduced tendency to dxidation
essential but mandatory to the production of a and to other deterioration. By these processes
grease suitable for the purpose desired. Due to it is possible to procure soaps of desired com
the varying types of oils employed in grease man positions in liquid condition by fusing the soap
ufacture, either in the soap for use in the grease under conditions which do not cause any sensi
or otherwise, accurate control of the glycerine ble decompositoin or deterioration. With the aid
content of lubricating greases has not heretofore of the molten anhydrous relatively pure soap it
been possible. , ". . . has been found possible to make intimate and
Having in mind the defects of the prior art 30 uniform mixtures of these soaps with other lu
methods and compositions, it is an object of the bricating grease materials which it is desirable to
invention to provide a new and improved method incorporate with them. I have found that this
of manufacturing lubricating greases. Another is made possible from the fact that the relatively
object of the invention is to provide new and - pure anhydrous Soaps in molten condition become
improved greases and lubricating compositions excellent solvents for many of these materials.
which give increased satisfaction in many places which at lower temperatures and in the presence
where lubricating compositions are now used or of a liquid water phase do not become dissolved
may be used. Another object of the invention therein, but merely emulsified therewith. It
is to simplify the manufacture of greases, while should be explained that the solvent action re
40 ferred to in the case of heated anhydrous ma
at the same time reducing the cost of manu
facture. Still another object is the provision of terials and anhydrous soap is a mutual one. For
a method for controlling unifornity and thus instance a melted anhydrous soap free from
superiority in lubricating compositions. Yet an water and glycerine will actually dissolve a high
other object is to provide a method for making 45 percentage of a high grade mineral lubricating
lubricating greases free from objectionable im oil without injuring it in any way, or conversely
purities such as grit, glycerine and water, common the mineral lubricating oil, being considered as
to most lubricating greases. - the solvent, dissolves a high percentage of an
Novel and unusual lubricating greases can be hydrous soap. At temperatures sufficiently high
prepared by my new and improved method by for fusion of pure anhydrous soap, as for example
combining in a molten state, anhydrous Soap Sub in the case of some soaps 290° C. to 300° C., the
stantially free of glycerine with mineral oil mutal solution of the anhydrous soap and the
and/or other lubricating adjuvants. The molten mineral lubricating oil is substantially in all
anhydrous soap substantially free of glycerine is proportions, whereas with the use of lubricating
advantageously prepared by the process described 55 oils thus dissolved with hot soap, a considerable
 2 2,319,405
percentage of both soap and oil being present, and a harder grease by the employment of more
there is a separation on cooling, to two phases, SO8.p.
the lower containing, when cold, the greater The process gives desirable results which are
concentration of soap and lesser concentration : surprising in the light of experience gained from
of the mineral lubricating oil, in some instances 5 ordinary greases. Thus, it is not customary to
as little as 20% of mineral oil, while the upper use much if any cocoanut oil in making lubricat
layer will comprise mineral oil to a larger de ing greases. This is because soap from this oil
gree and anhydrous soap to a lesser degree. is so soluble in Water and glycerine water, and is
It will be found that both of these layers, the () melted and dissolved so readily in these two
one richest in anhydrous soap and the one rich- ' inpurities that any ordinary lubricating grease
est in mineral lubricating oil, possess excellent containing water and glycerine and Cocoanut oil
properties as lubricating greases especially for soap would liquefy with rise in temperature in
severe duty requirements. Neither of these com use and separate and result in a broken film
positions will suffer physical or chemical break with inferior lubricating qualities. Also, cocoa
down under the most rigid requirements ordi nut oil yields 30% more glycerine than most other
narily met with in extreme cases. In any use at fats and oils and for this reason is not suitable
a temperature higher than that at which the two for use in ordinary greases made in known ways
phases separate there will be but one phase, said owing to the larger amount of glycerine that
single phase possessing good lubricating qualities. Would be left in Such greases.
The two phases may be kneaded together at low. 20 On the other hand, contrary to common belief,
temperatures with ease in the dry condition cocoanut oil soap when anhydrous and freed from
without addition, or with the incorporation of glycerine is appreciably higher melting than an
other lubricating material as for instance graph hydrous tallow Soap, for instance, or many other
ite and will make a Superior lubricating grease anhydrous Sodium soaps. Furthermore, anhy
consisting at Ordinary temperatures of two Solid 25 drous potash soaps are generally appreciably
phases (or in case graphite has been added, of higher melting than anhydrous sodium soaps
three solid phases). This physical condition will from corresponding fatty material. Potash soaps
give the composition a buttery, Smooth consistency have increased solubility in the presence of im
due to the tendency for one phase to slip against purities like water and glycerine with very much
the other and with no tendency for the grease to lowered melting points whereas the melting point
separate or change in an unfavorable manner due of the anhydrous potash soap free from glycerine
to increase in temperature, as rise in temperature is very high.
favors a mutual solution of the phases without
breakdown of the film of grease.
Soaps may also be made from material made in
accordance with my United States Patent No.
I may for example in preparing a lubricating s 1,951,511 issued March 20, 1934, or by making
arease in accordance with the invention take fattyhigher melting anhydrous soap with suitable
tallow or lard or horse fat or any of the fats or material mixed with a large proportion of
els commonly used for this purpose, or mixtures rosin. I have found that the melting points of
thereof, and make them into an anhydrous 40
Some of these anhydrous soaps made from oxi
sodium soap with the use of dry soda ash and dized petroleum compounds by the process of my
superheated steam agitation, at about 300° C. in United States Patent No. 1,951,511 are appre
the substantial absence of air or other deter ciably higher than the melting points of most
iorating influences, and thus obtain a pure soap anhydrous soaps made from natural fats, also
free from water and glycerine in thin molten that such anhydrous petroleum soaps have some
condition. As soon as the glycerine has been what lower melting points when made in the pres
removed, which takes but a comparatively short ence of, or when mixed with, certain high boiling
time, the desired amount, large or small, of a petroleum materials like high boiling mineral
desirable mineral oil constituent may be run into lubricating oils, there being at these high tem
the soap whereupon the two will mix rapidly and peratures a very considerable degree of mutual
: completely due to their substantially complete solubility. Also, anhydrous rosin soap made by
mutual solubility at the temperature employed. itself in the absence of fatty soaps or fluxing
The melting point of the grease thus formed is materials has a very high melting point com
lower than that of the pure anhydrous soap and pared with anhydrous soaps made from fats
it is therefore not necessary to maintain the same. 55 which generally melt around 300° C. if decom
high-temperature as in making the soap. After position is avoided.
the grease has thus been made, agitation may be Accordingly, the present invention permits of
stopped with reduction of temperature while ing the use of these high melting soaps while deriv
continuing to exclude air throughout the process comessignal advantages therefrom, as it thus be
possible to provide a plentiful supply of
as long as the grease is at a temperature above 60 inexpensive and at the same time superior high
the boiling point of water. A proper degree of viscosity greases for use in duty at high tem
subsidence will suffice to permit any chance peratures and particularly
objectionable solid or gritty impurities to settle where heavy loads must besuitable for such duty
continuously carried.
out so that with the use of a proper device the These products may be made by incorporating
grease may be run out free from such impurities. 65 high boiling lubricating materials at high tem
The grease may be run into a proper tank and peratures with these high melting soaps, taking
allowed to separate into two phases if desired, if proper precautions to thoroughly agitate the
its composition is such as to form such a separa heated mixture to avoid local overheating and to
tion, or it may be run at once to a cooling-mixer 70
thoroughly exclude air. Before beginning to chill
where it may be worked into a finished lubricant. the greases so made, grit and other insoluble solid
The process is very flexible while permitting matter should be separated and removed by sedi
accurate control of all steps and of the finished mentation or otherwise so that it may be ex
product. Thus a softer grease may be obtained cluded from the final product,
by employing a higher proportion of mineral oil, 75
It should be at once evident that the ordinary
processes of making greases in open greaseketles
 2,819,405 3
could not be employed at all for the manufacture from petroleum oils by fractional distillation are
of such high melting, high viscosity, high duty suitable; so also are mineral oil lubricants ob
greases, which by the present invention may be tained and purified from crude petroleum by sol
made without injury at temperatures that would vent extraction processes. Where greases are to
result instantly in fire if the air were not effec be employed for heavy duty and are required to
tively excluded. . . .... . . operate at high temperatures or to sustain great
These facts show how with the use of the loads it will generally be found desirable to em
present process and careful selection of materials ploy the higher boiling or the more viscous frac
employed, stable soaps and stable greases with tions of mineral oil and frequently desirable to
unusually high melting points suitable for very O pick a soap base with a higher melting point, and
heavy duty may be obtained, even from those in all cases it is desirable to choose a composi
2... materials previously considered wholly unsatis tion that will not give a two phase separation in
factory for Such purposes. use, with two quite dissimilar phases, SO that an
Lubricating greases are put to a great Variety easily ruptured film will result and cause wear
of uses and some greases are more suitable than ing surfaces to come into actual contact with
others for some uses. For SOme purposes a grease one another and even to "seize.'
containing lime soap, or calcium Soap, Will be For some uses, requirements are quite opposite
found to be better than one made with a sodium from others. Thus, for lubricating curved rails
or potash soap. The present process lends it to prevent flange friction, waterproof qualities are
self readily to the making of a soap with almost desirable so that the grease will not become de
any desired base or bases. Thus for making a tached by rain or snow; a more or less permanent
calcium soap from tallow I may mix with each consistency is desirable even. On long exposure SO
100 lbs. tallow about 50 lbs.good quality pulverized that the grease will continue to function, and it
limestone and treat the mixture with superheated must also display reasonably good lubricating
steam at about 300° C. in such a Way as to ex 25 qualities though certainly not the same as a grease
clude air, prevent local overheating, and distill off used to lubricate a heavily loaded bearing hous
and collect the glycerine formed. For this pur ing, or a rapidly revolving axle, or a wrist pin.
pose I may employ controlled indirect heating as A good cheap grease may be made by the present
for instance diphenyl vapor under pressure, or invention with a cheap fatty matter mixed with
diphenyl oxide vapor, or a mixture of the two. In 30 cheap rosin to make an anhydrous soap which
this way I may obtain a purer more completely may be mixed with cheap petroleum products
saponified calcium soap than may be obtained by such as still tar or fuel oil or even with Some
ordinary processes, and one free from the ob asphalt and cheap oil, M
jectionable impurities, water and glycerine, and For some purposes materials other than the
because of the fluidity of the Soap I may free it 35 ordinary soap-making materials may be emi
completely from gritty impurities in a Way that is ployed in the process to advantage as for instance
not possible with ordinary calcium soaps and naphthenic acid neutralized by the process with
calcium soap greases. Calcium Soap grease pre a suitable base, or used in conjunction with fatty
pared by the present process with the aid of Suit or rosin matter. Tall oil, Waxes and Wool fat
able mineral lubricating oil, e. g., 70%, 80%, or 40 soaps may also be used advantageously by the
90% of a lubricating oil possessing a Saybolt vis present novel process for some types of lubricat
cosity of 180-200 at 100°F, have special advan ing greases. I may make good greases by the
tages for many purposes. For instance When present process using fatty acids with complete
prepared with proper consistency it is very Well conversion of their acid qualities to "neutral'
suited as a cup grease and it may be used both greases. Lubricating greases may be used with
as a stiff and as a soft grease With grease guns. or without addition of graphite, chlorinated hy
It is very suitable as a water proof grease for use drocarbons, or the like. Greases made with one
in cups lubricating water pumps or pumps for class of materials may be blended With greases
other liquids, and is especially well suited to lubris made from other materials.
cate outboard bearings of propeller shafts. 50 The process may be modified by making the
It is riot generally feasible to use other bases soaps by some other method of saponification and
thah the alkalies and calcium or mixtures there then purifying the soap thus made by the heat
of, though some others like aluminum and lead steam treatment before making the final lubri
are worked iro greases with difficulty. The cating grease. Although there is no special ad
present invention enables one to make special vantage in doing so, the Saponification may be
greases with greater ease than they may other performed in the presence of Some of the mineral
wise be made. I may for instance readily make oil product. The melt thus formed is lower melt
a magnesium soap grease and find it especially ing than the one from pure soap but on the other
easy to make a calcium-magnesium Soap grease hand. Some of the mineral oil product Will distill
that has its own characteristic advantages, by 60 over with the steam and Will have to be col
employing a good grade of pulverized dolomite in lected to avoid loSS, and the greater advantage
proper amounts with a desired fatty material. is obtained when very little of the mineral oil
Under the conditions which are well suited for product is distilled over.
this type of manufacture the saponification may Greases made by the present invention, Owing
be carried out in a still-like vessel with direct 65
to the absence of water and glycerine and objec
steam agitation at about 300 C. With of without tionable acid impurities, exert practically no cor
vacuum so as to distill off the glycerine and pre rosive qualities on metals On Which they are used
vent local overheating. The mixed calcium at any temperature, though Such action is a con
magnesium soap melts with even greater ease
than the calcium soap alone, and when incorpo 70 mon fault of many ordinary greases.
rated with propermineral oil lubricating fractions While I have illustrated my invention with
makes a very satisfactory grease. Specific examples, it is to be understood that it is
one may have great leeway in selecting the not to be restricted thereto, but is to be inited
mineral oil constituent for these greases accord Only by the broad principles of the disclosure and
ing to their intended uses. Fractions obtained 75 by the claims.
4. 2,819,405
claim: of forming two separate grease phases upon cool
1. The process of manufacturing lubricating ing, agitating and maintaining a temperature
grease which comprises making a substantially above about the melting point of the anhydrous
pure anhydrous soap in molten condition Sub Soap during Said mixing to produce a high degree
stantially free from glycerine, unsaponified, and of fluidity and mutual solubility of said soap and
volatile unsaponifiable matter, grit and other said lubricant in the mixture, cooling said mix
impurities, and mixing therewith a mineral base ture without harmful exposure to air, and stir
lubricating material while the two are in a Sub ring during cooling to prevent segregation of said
stantially fused anhydrous condition, with sub grease phases.
stantial absence of air, and cooling the product 6. A lubricating grease Substantially free from
with stirring with substantial absence of air. water, glycerine, volatile impurities and grit,
2. The process of manufacturing lubricating comprising a mineral oil lubricant, calcium and
grease which comprises saponifying a fat or fatty magnesium Soaps, the calcium and magnesium
oil with a base and heating the mixture thus Soaps being in approximately the same relative
formed with the aid of thorough agitation and proportions as the calcium and magnesium oc
flow of steam and substantial exclusion of air to Curring in dolomite limestones.
a temperature in excess of the melting point of 7. The process of manufacturing lubricating
the resulting anhydrous Soap, volatilizing there greases which Comprises the joint incorporation
from the glycerine that is formed, while con therein, in the absence of liquid water and glyc
tinuing the agitation, flow of Steam, and exclu 2) erine, of a mineral oil lubricant and of a high
sion of air, and mixing with the resulting molten melting anhydrous soap made from oxidized
anhydrous soap in the Substantial absence of air petroleum hydrocarbons, said anhydrous soap
a high boiling mineral lubricating oil which is having been modified by subjection to a tempera
appreciably mutually soluble with said soap at ture above about the melting point of the an
the temperature employed for Said mixing, and 25 hydrous Soap and to thorough agitation in the
cooling the product with stirring. absence of air with the aid of a current of steam
3. The process of making lubricating greases for a period of time sufficient to effect the sub
which comprises intimately mixing in the sub Stantial removal of the hydroxyl groups from
stantial absence of air a fused anhydrous soap hydroxy Soaps therein.
made from coconut oil and Substantially free from 3) 8. The process of manufacturing lubricating
glycerine with a high-boiling mineral lubricating greases which comprises the joint incorporation
oil.
4. The process of making lubricating greases therein, at elevated temperatures and above the
melting temperature of said greases in the sub
which comprises mixing at a high temperature stantial
with the exclusion of air, a Soap Substantially 35 ties and absence of liquid water, volatile impuri
glycerine, of a high melting anhydrous
free of water, volatile impurities and glycerine rosin Soap and a high boiling lubricating mate
with a mineral oil lubricant in such proportion rial.
that said soap and Said lubricant have a high '9. A lubricating grease substantially free from
degree of mutual solubility under the mixing con Water, glycerine, volatile impurities and grit,
ditions and in such proportion that the product 40 comprising a mineral oil lubricant and an an
thereof will form two separate grease phases hydrous Soap made by oxidation of petroleum
upon cooling, agitating and maintaining a ten hydrocarbons, which Soap has been subjected to
perature above about the melting point of the a temperature above about the melting point of
anhydrous soap during said mixing to produce a the anhydrous Soap, in the absence of air, for a
high degree of fluidity and mutual solubility of period of time Sufficient to effect the substantial
said soap and Said lubricant, cooling Said mix removal of the hydroxyl groups from hydroxy
ture without harmful exposure to air to form Soaps therein.
two grease phases, and Separating the two grease 10. A lubricating grease substantially free from
phaSeS.
5. The process of making lubricating greases 50 Curringgrit,
Water, glycerine and volatile impurities oc
in fats and fatty oils, comprising mineral
which comprises mixing at a high temperature lubricating oil and anhydrous soap made from
in the substantial absence of air, a Soap Substan naturally-occurring glycerides, which soap has
tially free of water, volatile impurities and glyc beer. Subjected to a temperature at least as high
erine with a mineral oil lubricant in Such propor as the melting point of the anhydrous soap, in
tion and at such temperature that Said Soap and 55 the absence of air, for a period of time sufficient
said lubricant have a high degree of mutual Solu to reduce the tendency of the soap to oxidize and
bility under the mixing conditions and in such otherwise to deteriorate.
proportion that the product thereof is capable VARTIN HILL TTNER.
 - CERTIFICATE OF CORRECTION.
Patent No. 2,319,405. . May 18, 1943.
MARTIN HILL, ITTNER

It is hereby certified that error appears in the printed specification

Henry Wan. Arsdale,