IMPROVE- MENTS IN TREATING FATTY, OILY, Waxy, and Hydrocarbon BODIES
Year: 1871

page_text: LETTERS PATENT to George Gwynne, of Marylebone Road, in the
County of Middlesex, Gentleman, for the Invention of "IMPROVE-
MENTS IN TREATING FATTY, OILY, Waxy, and Hydrocarbon BODIES.”
"
MENTS IN TREATING FATTY, OILY, Waxy, and HydROCARBON BODIES.”
PROVISIONAL SPECIFICATION left by the said George Gwynne at the
Office of the Commissioners of Patents, with his Petition, on the
26th June 1871.
I, GEORGE GWYNNE, of Marylebone Road, in the County of Mid-
5 dlesex, Gentleman, do hereby declare the nature of the said Invention
for "IMPROVEMENTS IN TREATING FATTY, OILY, WAXY, AND HYDROCARBON BODIES,"
to be as follows :-
It is a fact well known to chemists that liquids will readily part with
their impurities by simple filtration when presented to the filtering
O medium in a sufficiently thin or diluted state.
Now the object of the present Invention is to render available this
knowledge for the treatment of fatty, oily, and waxy bodies, and also

page_text: of certain hydrocarbons, and thereby to prevent the necessity of sub-
jecting these substances to high temperatures, which change their
quality and add greatly to the cost of the purifying process. Some of
the substances which it is proposed to treat are solid at atmospheric
temperatures, and these it is necessary to melt before treating them.
according to this Invention. In other respects the process of puri-
fying them will be substantially the same as that used for hydrocarbon
oils.
The solid substances which it is proposed to treat may be represented
by beeswax, vegetable wax, earth wax, and crude paraffin, and the liquid
substances by palm oil, rape oil, and the fixed oils generally.
The substantial feature of the Invention applicable alike to all those
substances, is the thinning or dilution of the same by some suitable
volatile solvent, and submitting the same when diluted to a charcoal or
other filter.
The following are examples which will suffice to explain the manner
of treating the above-mentioned substances.
The treatment of earth wax may be taken as an illustration of the
mode of dealing with the solid substances. Hitherto this material has
been subjected to distillation and pressure in order to render it available a
for use in the arts. It is now proposed to place a quantity of this sub-
stance in an open pan provided with a steam jacket, connected with a
high-pressure steam boiler, and to raise the temperature to about 212°
and then thoroughly to incorporate into it so much of a strong solution
of caustic soda as will entirely remove all impurities precipitable by that
agent. After about two hours stirring, the matters under process are
allowed to repose that the impurities may subside. The supernatant
"earth wax" is then drawn off into a closed vessel containing an agitator,
and to it is then added as much of the volatile solvent as will prevent
the "earth wax " from solidifying until the temperature has fallen to
about 100°. The temperature of the mixture is then raised to about 120°
and treated three or four times with small doses of concentrated sulphuric
acid, the precipitate being drawn off after due subsidence following
cach acid treatment. The matter under process is then washed with
tepid water until the whole of the adhering acid is removed. The dilute
earth wax is then allowed to repose, until it has become clear, and it is
next passed in a heated state through a closed filter of animal charcoal
similar in size and composition to those used by sugar refiners of the

page_text: present day. The dilute state of the liquid will render it unnecessary
to raise it to a high or injurious temperature to ensure its passing freely
through the filter. The filtered mixture as it leaves the filter may bo
received into a suitable still to drive off the volatile solvent which when
condensed may be used again as before.
•
For the purification of the liquid substances such as rape oil the
process will be similar to that given for the earth wax, with these
exceptions that carbonate of soda is used in place of caustic soda and
diluto sulphuric acid in place of concentrated sulphuric acid. The
solvent also will be less in proportion for the liquid than for the solid
substances treated. It may be here remarked that the treatment with
the alkalies and acids is adopted mainly for the purpose of economising
the filtering material as they serve to remove impurities which would
otherwise pass to and be retained in the filter, and would thereby rapidly
deteriorate the efficiency of the filtering material. The solvents used
may be naptha, turpentine, or bi-sulphide of carbon.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said George Gwynne in the Great Seal Patent Office
on the 23rd December 1871.
TO. ALL TO WHOM THESE PRESENTS SHALL COME, I, GEORGE
GWYNNE, of Marylebone Road, in the County of Middlesex, Gentleman,
send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twenty-sixth day of June, in the year
of our Lord One thousand eight hundred and seventy-one, in the thirty-
fifth year of Her reign, did, for Herself, Her heirs and successors,
give and grant unto me, the said George Gwynnc, Her special licence
that I, the said George Gwynne, my executors, administrators, and
assigns, or such others as I, the said George Gwynne, my executors,
administrators, and assigns, should at any time agree with, and no
others, from time to time and at all times thereafter during the term
therein expressed, should and lawfully might make, use, exercise, and
vend, within the United Kingdom of Great Britain and Ireland, tho
Channel Islands, and Isle of Man, an Invention for ** IMPROVEMENTS
IN TREATING FATTY, Oily, Waxy, and HYDROCARBON BODIES," upon the con-

page_text: dition (amongst others) that I, the said George Gwynne, my executors or
administrators, by an instrument in writing under my, or their, or one
of their hands and seals, should particularly describe and ascertain the
nature of the said Invention, and in what manner the same was to be
performed, and cause the same to be filed in the Great Scal Patent
Office within six calendar months next and immediately after the date
of the said Letters Patent.
NOW KNOW YE, that I, the said George Gwynne, do hereby declare
the nature of my said Invention, and in what manner the same is
to be performed, to be particularly described and ascertained in and by
the following statement (that is'to say) :-
It is a fact well known to chemists that liquids will readily part with
their impuritics by simple filtration when presented to the filtering
medium in a sufficiently thin or diluted state.
Now the object of the present Invention is to render available this
knowledge for the treatment of fatty, oily, and waxy bodies, and also of
certain hydrocarbons, and thereby to prevent the necessity of subjecting
these substances to high temperatures, which change their quality and
add greatly to the cost of the purifying process. Some of the substances
which it is proposed to treat are solid at atmospheric temperatures, and
these it is necessary to melt before treating them according to this
Invention.
The solid substances which it is proposed to treat may be represented
by beeswax, vegetable wax, earth wax, crude paraffin, tallow, and palm
oil, and the liquid substances by olive oil, rape oil, and the fixed oils a
generally.
The substantial feature of the Invention, applicable alike to all these
substances is, the thinning or dilution of the same by some suitable
volatile solvent, and submitting the diluted substances to a charcoal or
other filter.
I find that fatty, oily, waxy, and hydrocarbon bodics. contain certain
impurities which it is advantageous to remove before the filtration
through charcoal takes place, and as the same treatment for the removal
of these impurities is not equally suitable for all of them, a few details
upon this point may be advisable. I shall begin with,-
possesses
Earth wax. This substance is very similar to paraffin, but it
a much higher melting point than that body. Strong solution of caustic
3
3

page_text: soda and concentrated sulphuric acid which are so largely used by the
shale oil refiner are quite thrown away upon this intractable substance.
The preparatory process for it preceding dissolution in the solvent which
has been found to answer may be thus described:-The earth wax is well
agitated at the temperature of two hundred degrees for four hours in a
weak solution of caustic soda, allowed to settle, and then transferred into
another pan provided with a steam jacket and lined with sheet lead.
In this vessel it is agitated for six hours with dilute sulphuric acid.
During which time the temperature of the mixture should be kept at
about two hundred degrees Fahrenheit. At the end of the six hours
the matters under process should be allowed to settle, when the super-
natant earth wax is to be removed into an ordinary boiling tub,
provided with a copper free steam worm, and boiled for one hour in its.
own bulk of water. As the earth wax has a very high melting point, a
small jet of steam should be allowed to play into the steam jackets
during the settlings so as to maintain the temperature near to but not so
high as two hundred degrees.
The solution of caustic soda used here is of the specific gravity of one
thousand and fifty, at the temperature of sixty degrees, and the quantity
employed is at the rate of seventy-five gallons for each ton of earth wax
under treatment. The sulphuric acid solution is made by adding eighty
pounds of concentrated sulphuric acid to eighty imperial gallons of
water, and this quantity is sufficient for a ton of earth wax.
Beeswax, vegetable wax, and other bodies of this kind, are not to be
treated with soda at all in the preparatory process; they are merely to
be boiled with very dilute sulphuric acid for an hour in an ordinary
boiling tub provided with a free steam worm. The quantity of sulphuric
acid here used is twenty pounds of concentrated acid and one hundred
imperial gallons of water for each ton of beeswax.
Crude paraffin.-A strong solution of caustic soda and concentrated
sulphuric acid are agents constantly and largely employed in the refining
of this substance, and there can be no question as to their beneficial
effects. But they have their disadvantages, for while removing im-
purities they carry away also matters that should be left behind, and
I do not therefore use them; but instead thereof I employ a weak
solution of caustic soda and dilute sulphuric acid. The soda solution
used for this substance is of the gravity of one thousand and fifty, at the
temperature of sixty degrees Fahrenhoit, and the sulphuric acid solution

page_text: is made by adding one part by weight of concentrated acid to four parts
by weight of water.
The mode of using these agents is as follows:-The crude material in
the first instance is put into an iron pan provided with a steam jacket,
and as much soda solution is added as will carry down all the impurities 5
removeable by that agent. The steam is then let into the jacket and
the temperature raised to about two hundred degrees Fahrenheit, and
kept up for about four hours, stirring being maintained all the time.
The matters under process are then allowed to repose until the soda
and impurities have settled to the bottom of the vessel, the clean 1
material is then to be transferred into another pan lined with sheet
lead and provided with a steam jacket, where it is treated with the
sulphuric acid solution and kept in this pan at the temperature of about
one hundred and forty degrees Fahrenheit for about six hours with
constant stirring. The quantities of soda solution and acid solution here 1
employed will somewhat vary, depending upon the amount of impurities
existing in the crude material, but a little experience will quickly point
out the right proportions to be employed. The plan which I pursue is
to take up some of the mixture in an evaporating basin, allow it to
settle for a while, then pour a portion of it into a test tube, and try it 2
with the dilute acid or the soda solution, as the case may be. If neither
of these agents produces any effect I consider enough has been used.
If, on the contrary, an effect is produced, I use more of the acid or soda
solution, as the case may be. After the crude paraffin has been treated
with dilute sulphuric acid, in the manner described, and allowed to 2
settle, it is boiled in an ordinary boiling tub, provided with a free steam
copper worm in its own bulk of plain water for an hour.
Tallow, palm oil, rape oil, and other natural fatty and oily matters,
are to be treated with alkalics or carbonated alkalies in the preparatory
process, and with diluted sulphuric acid before being dissolved in or
diluted by the volatile solvent. As far as my experience goes, car-
bonated alkalies are superior for the purpose here indicated to caustic
alkalies; and of the carbonated alkalies I prefer to employ the ordinary
crystallized carbonate of soda. As the purification of fatty and oily
matters by alkalies and carbonated alkalies are known processes, it is 3
not necessary for me to describe them here.
The tallow, palm oil, rape oil, &c., as the case may be, having been
purified with carbonate of soda, is then. treated with the dilute sulphuric

page_text: acid in a manner similar to that described for crude paraffin, washing
included, with the following exceptions, viz. :-The sulphuric acid
solution is composed of forty pounds of concentrated sulphuric acid,
and eight imperial gallons of water. This quantity is sufficient for
one ton of the material to be operated upon, and the temperature of the
solution is to be maintained at one hundred and twenty degrees instead
of one hundred and ten degrees Fahrenheit.
The substances which it is proposed to treat by this Invention having
been subjected to the preparatory processes herein set forth are next to
be thinned or diluted by the volatile solvent to facilitate their filtration.
The vessel in which this operation is to be performed should be a close
one to prevent any escape of the volatile solvent, and should be provided
with a mechanical agitator, a small stop-cock to draw off samples, a
thermometer, and a steam jacket. This jacket should be so arranged
that either cold water or steam can be admitted into its interior at
pleasure. As the solvent boils at a low temperature, and is to be used
over and over again the amount employed to thin or dilute the different
materials is of little consequence, provided there is sufficient for the
purpose.
When earth wax is the material to be operated upon I run into the
dissolving vessel a quantity of the solvent in a cold state, and the
mechanical agitator being set in motion I admit the earth wax slowly
in a melted state until the solvent is fully saturated with it at the
temperature of about eighty degrees Fahrenheit. A slight excess of
the earth wax is unimportant. From the stop-cock in the side of
the vessel a sample can be taken out from time to time to ascertain
how the saturation proceeds. As the earth wax has a very high melting
point, and will convey a great amount of heat into the solvent, the
thermometer should be examined from time to time to see that the
temperature does not rise above eighty degrees Fahrenheit. Should
this event occur, the flow of the melted earth wax should be either
slackened or stopped altogether for a time, and cold water admitted
into the jacket. When the saturation of the solvent at about eighty
degrees Fahrenheit has been accomplished, the contents of the dis-
solving vessel are to be run into a large and close tank or vat, and
a fresh charge of the solvent and earth wax is let into the dissolving
vessel, and so on until the tank is full. The tank should be placed in a
room or building, the temperature of which should be maintained at
.

page_text: about eighty degrees Fahrenheit. The matters in the tank arc to bo
allowed to repose until the solution of the carth wax has become bright,
after which it is to be run into the charcoal filter.
Beeswax, vegetable wax, and such like matters, are to be treated in
the dissolving vessel and settling tank, in the manner just described for
earth wax.
Crude Paraffin.-In operating upon this body it is preferred to have
more of the solvent than is required to hold it in solution. Four parts
by weight of the solvent to one part by weight of the crude paraffin aro
suitable proportions. The temperature of cighty degrees Fahrenheit
should be attended to as before mentioned, both in the dissolving vessel
and in the settling tank.
Tallow, palm oil, rape oil, and other fatty and oily matters.-The
directions previously given for crude paraffin answer for these substances
very well.
The filtration.-The charcoal filters which are proposed to be used in
carrying out this Invention are somewhat similar to those employed by
the sugar refiner, with the exception that they have closed tops to
prevent the loss of the volatile solvent. The covers of the filters may be
taken off or screwed down quite tight as required. A charcoal filter, a
seven feet deep and four fect in diameter, is a suitable size for the
purpose; a filter of these dimensions will conveniently give a depth of
six fect of charcoal. This material should be coarse grained, precisely
similar to the sugar house charcoal. A vacant space between the cover
and the charcoal is to be left to enable the solution to distribute itself
properly through the charcoal, and also to enable steam (the use of
which will be presently explained) to permeate freely through the
charcoal. A set of filters of this kind being provided there will be
required besides three or four closed cisterns and two stills with con-
densers. The filters should be placed in a warm room or building kept
at the temperature of about one hundred degrees Fahrenheit.
I will now describe the mode of working :-From the settling tank
before mentioned the volatile solution containing carth wax or any of
the other substances set forth-in the description of this Invention is to
be allowed to flow into the charcoal filter. The cock at the botton of
this vessel is to be kept shut until the solution has descended to the
bottom of the charcoal when the cock is to be opened, but not to its
full extent, the object being to allow the solution to flow only slowly

page_text: through the charcoal. At first the solution is a little muddy from
suspended particles of charcoal, but this soon ceases if the filter has
been properly packed. The muddy solution is to be let into a cistern
specially reserved for it, from whence it is to be again pumped upon the
top of the charcoal. When the solution runs clear it is to be let into
one of the stills, and so soon as a sufficient quantity has accumu-
lated therein (say the amount equal to half the capacity of the still)
free steam is to be admitted thereto through a properly constructed
distributing worm, the filter meantime continuing the supply. Shortly
after the introduction of the steam the volatile solvent will begin to
vaporizo and pass off into the condenser, where it is condensed, and
whence it will flow into a receiving cistern ready to be again used on
fresh materials in the dissolving vessel. As soon as a considerablo
quantity of the earth wax or other material under treatment has accu-
mulated in the still, and the solvent accompanying it has been driven
off by the steam, the material is to be discharged into a suitable vessel,
from which it may be taken for the purposes required.
As the final disposal of the substances forms no part of this Invention,
it is unnecessary to say more upon this point. Although the solution
runs colourless from the filter for a time, it at last begins to acquiro
a tint, which gradually increases until the solution becomes as dark
as it was before it entered the filter, that is provided the flow of the
solution is continued long enough. The solution begins to get coloured
long before the strength of the charcoal is exhausted, and the most
economical plan in this case is to let into the stills only so much
as is of good colour, and allow the remainder of the solution to run
through the filter until the charcoal is nearly exhausted of its deco-
lourizing property, and then to pass it over a fresh filter of charcoal
to complete the filtration.
When the decolourizing power of the charcoal is nearly exhausted
the solution still remaining on the charcoal is to be forced out by
means of steam introduced through the closed cover. After the steam
has performed this duty and the charcoal has become sufficiently cool,
the cover is to be removed, the charcoal taken out and reburned, after
which it may be used over again, and so on.
I wish it to be understood that I do not limit myself to the use of any
particular volatile solvent. I prefer to use either bisulphide of carbon
or petroleum spirit. When I use the latter, I prefer to redistil it before

page_text: employing it as the solvent or diluent for the substances set forth in the
description of this Invention.
Having now set forth the nature of the said Invention, and explained
the manner of carrying the same into effect, I wish it to be understood
that under the above in part recited Letters Patent I claim, filtering
fatty, oily, waxy, and hydrocarbon bodies with the aid of a volatile
solvent or diluent, in the manner and for the purpose above described.
In witness whereof, I, the said George Gwynne, have hereunto set
my hand and seal, the Twenty-second day of December, in the
year of our Lord One thousand eight hundred and seventy-one.