AN IMPROVED PROCESS FOR IMPROVING OR INCREASING THE VISCOSITY OF OILS
Year: 1885

page_text: We, WILLIAM MARRIOTT and HENRY MARRIOTT of the firm of William Marriott
and Son of the Leeds Road Chemical Works, Huddersfield, Yorkshire Manu-
facturing Chemists, do hereby declare the nature of our invention for "
AN
IMPROVED PROCESS FOR IMPROVING OR INCREASING THE VISCOSITY OF OILS " to
be as follows:-
The object of this Invention is to increase the viscosity or tenacity of lubricating
oils, mineral or otherwise, and this we effect by adding to, or combining with the
said oils oleate and stearate of alumina.
The proportion of aluminate which is to be added to, or combined, with the
oils depends upon the degree of viscosity required, but five per cent of pure
aluminate will give a good average lubricating oil.
The production or separation of oleic, or stearic acid from tallow and oil is well
known and understood, being extensively carried on in the manufacture of candles,
which oleic or stearic acid may be converted into oleate and stearate of alumina
for mixing with oils so as to increase their viscosity according to our invention, but
we prefer to obtain the oleic or stearic acid from a cheaper source than that of
tallow or oil.
For this purpose we make use of the dark semi-solid grease or black oil herein-
after called "brown grease" which is recovered by any well known process from
greasy shoddy, or the water used in scouring off the soap or oil used in the
manufacture of woollen or worsted goods wool washing, or the "foots" made in
refining vegetable or animal oils,
a
In treating the
brown grease
" for the purpose of extracting the oleic and
stearic acid we place it into a metal still partially heated by fire, and also by
superheated steam which enters into the said still near the bottom thereof by
means of a pipe terminating in a rose, the steam thus introduced passes up through
the brown grease, which in addition to the heat from the fire, will gradually bring
the temperature up to the point at which the oleic and stearic acid passes away
along with the steam, which together are led by a pipe into a vessel technically
Called a **
worm or coil and there condensed and as water is the heavier body it
"

page_text: soon settles to the bottom of the receiver where it is easily separated from the oleic
and stearic acids; we do not however use the portion first condensed as it contains
a little volatile spirit of a disagreeable odour, neither do we use the latter portion
as it is of a dark colour but preferably we collect so much as is of a good colour,
whilst the remainder is added to the next charge of grease put in the still, and the
pitch which is found in the still after such charge is drawn off, may be used for
other purposes.
The oleic and stearic acids obtained as above described vary a little in their
proportions to each other, but they answer well for the purpose which we will now
describe.
The oleic and stearic acid is now converted into oleate and stearate of alumina,
which for the sake of brevity we will call the substance oleate of alumina, though
stearic acid forms part of the combination.
Before conversion into aluminate it is necessary to ascertain the weight of dry
pure caustic soda required to saturate-say 100 parts by weight of the mixed oleic
and stearic acids, this will be found to be about 10 per cent, but in practice a
little more say about per cent more is desirable to prevent waste of oil.
The proportions of materials used are 100 parts by weight of oleic and stearic
acid 10 parts dry caustic soda of 100 per cent and 50 parts of alum.
We do not
however restrict ourselves to these proportions, but we find them to give good
results. An iron pan with a hemispherical bottom, and a discharge pipe from the
same is a very convenient apparatus for the purpose of this conversion into
aluminate, and is best heated by a coil of lead pipe laid in the bottom of the
said pan.
We now place in the pan 400 parts of water and to that add 50 parts of alum,
and when dissolved add the 100 parts of oleic and stearic acid, which must be
heated to the boiling point and when in strong ebullition run in very gradually
the caustic soda, which must previously have been dissolved in such a quantity of
water as to stand at 17 Twaddle's Hydrometer.
The contents of the pan must be well agitated during the addition of the caustic
Boda, as the aluminate floats on the surface during its formation, and when the
solution of alum assumes a milky appearance it shews that sufficient caustic soda
has been added. The boiling must however be continued until the oleate of
alumina assumes a gelatinous form, and the milky appearance of the solution must
remain permanent.
The steam may then be shut off from the coil, when the contents will quickly
separate; this solution may afterwards be run off and the pan filled with fresh
clean water, and again boiled for some little time and this operation must be
repeated until the water from the pan runs off clear. In this state the aluminate
left in the pan contains a little water, but this is gradually expelled by heating it
along with the oil (required to have its viscosity increased) to a temperature of
about 212 Fahranheit and retained at the same temperature until the oil becomes
bright,
:

page_text: An Improved Process for Improving or Increasing the Viscosity.
of Oils.
We, WILLIAM MARRIOTT and HENRY MARRIOTT of the firm of William Marriott
and Son of the Leeds Road Chemical Works, Huddersfield, Yorkshire Manu-
facturing Chemists, do hereby declare the nature of our invention for "AN
IMPROVED PROCESS FOR IMPROVING OR INCREASING THE VISCOSITY OF OILS," and
in what manner the same is to be performed, to be particularly described and
ascertained in and by the following statement :-
The object of this invention is to increase the viscosity or tenacity of lubricating
oils, mineral or otherwise, and this we effect by adding to or combining with the
said oils oleate and stearate of alumina.
The proportion of salt of aluminium which is to be added to or combined with
the oils depends upon the degree of viscosity required, but five per cent of pure
aluminate will give a good average lubricating oil.
The production or separation of oleic or stearic acid from tallow and oil is well
known and understood being extensiveley carried on in the manufacture of candles,
which oleic or stearic acid may be converted into oleate and stearate of alumina
for mixing with oils so as to increase their viscosity according to our invention, but
we prefer to obtain the oleic or stearic acid from a cheaper source than that of
tallow or oil,
For this purpose we make use of the dark semi-solid grease or black oil, herein-
after called "brown grease" which is recovered by any well known process from
greasy shoddy, or the water used in scouring off the soap or oil used in the
manufacture of woollen or worsted goods, wool washing, or the "foots" made in
refining vegetable or animal oils.
"
In treating the brown grease for the purpose of extracting the oleic and stearic
acid, we place it into a metal still partially heated by fire, and also by superheated
steam which enters into the said still near the bottom thereof, by means of a pipe
terminating in a nose, the steam thus introduced passes up through the brown
grease, which in addition to the heat from the fire will gradually bring the tem-
perature up to the point at which the oleic and stearic acid passes away along with
the steam which together are led by a pipe into a vessel technically called a
"worm or coil and there condensed, and as water is the heavier body it soon
settles to the bottom of the receiver where it is easily separated from the oleic and
stearic acids; we do not however use the portion first condensed as it contains a
little volatile spirit of a disagreeable odour, neither do we use the latter portion as
it is of a dark colour, but preferably we collect so much as is of a good colour
whilst the remainder is added to the next charge of grease put in the still; and the
pitch which is found in the still after such charge is drawn off, may be used for
other purposes.
The oleic and stearic acids obtained as above described vary a little in their
proportions to each other, but they answer well for the purpose which we will now
describe.

page_text: ་
The oleic and stearic acid is now converted into oleate and stearate of alumina,
which for the sake of brevity we will call the substance oleate of alumina, though
stearic acid forms part of the combination.
Before conversion into salts of aluminium it is necessary to ascertain the weight
of dry pure caustic soda required to saturate-say-100 parts by weight of the
mixed oleic and stearic acids this will be found to be about 10 per cent, but in
practice a little more say about per cent more is desirable to prevent waste of
oil. The proportions of materials used are 100 parts by weight of oleic and stearic
acid, 10 parts of dry caustic soda of 100 per cent, and 50 parts of alum.
We do not however restrict ourselves to these proportions, but we find them to
give good results. An iron pan with a hemispherical bottom and a discharge pipe
from the same is a very convenient apparatus for the purpose of this conversion
into aluminate, and is best heated by a coil of lead pipe laid in the bottom of the
Baid pan.
This pan should be provided with an agitator and driven by power, one with
two horizontal arms through which are passed perpendicular bars; two inches
broad and two inches apart we find make a good agitator,
We now give the mode of working we have found to produce good and uniform
results.
Place in the pan 400 parts of water, and when boiling run in 100 parts of oleic
and stearic acid, which when come up to the boiling temperature gradually run
in 10 lbs of caustic soda of 100 per cent previously diluted to 20 degrees
twaddle.
This must be allowed to boil until the oleic and stearic acid is fully converted
into soap, a little experience will now enable an intelligent workman to judge the
time necessary. The soap begins to aglutinate together and if any smooth body-
say a knife blade be dipped therein it will be found to part in places from the
metal.
It must now be tested to see if there is an excess of caustic soda, this being
necessary to prevent waste of oil.
We use phthalic phenole as a test for this purpose, which gives a deep crimson
colour, if caustic soda is in excess even in a dilute solution. After this we add the
alum 50 parts previously dissolved in water, whilst the alum is being introduced
we shut off the steam from the pan, when the mass will gradually assume a curdy
appearance and the water will part from the salts of aluminium.
The steam may now be turned on, and the substances heated to the boiling
temperature and should be continued from one to two hours, when the salts of
aluminium will gradually assume a thick gelatinous appearance. If the steam is
shut off now and the substance allowed to be at rest for about 20 minutes, the
solution containing the soluble salts formed by decomposing the soda soap with
alum may be drawn off, first testing a portion of the liquid with ammonia, and if a
flacculent precipitate forms it is evident that sufficient alum has been used, if not,
more alum solution must be added.
The solution may now be run off, and the pan filled up with clean water, and
brought up to the boiling temperature.
This working must be repeated until the water runs off clear, and does not give
a precipitate with ammonia.
The salts of aluminium left in the pan still contain a portion of water, to expel
which the steam may be superheated up to 300 degrees. When thoroughly freed
from moisture the salts of aluminium when cold is a tenacious solid; which it
would almost be impossible to remove from the pan.
To obviate this we add whilst the salts of aluminium are still hot, four parts
of 905 mineral oil to one of salts of aluminium, which are agitated together until
of a uniform consistency. In this state it is run into casks which we prefer to
call viscom.
This viscom may be added to any oil to increase its viscosity which is done at a
temperature of 212 degrees agitating the two together,

page_text: If oleic acid alone is used the viscom is of a semi-solid, if stearic acid be used
the viscom is solid when cold.
By varying the proportions of the two acids, any intermediate consistency may
be obtained.
Having now. described the nature and particulars of this our Invention, and
the manner in which the same may be performed and carried into practice, we
would observe that we do not limit ourselves to any of the proportions herein
mentioned, nor to the manner of working, as such may and will vary, but what we
claim as our invention is;
The combination with mineral or other lubricating oils of oleate and stearite of
alumina, for increasing the viscosity or tenacity of the said oils.
WILLIAM MARRIOTT.
HENRY MARRIOTT.