IMPROVEMENTS IN The PROCESS FOR EXTRACTING OILS BY DIFFUSION AND IN THE PREPARATION Of MATERIALS AND ARRANGEMENT OF APPARATUS FOR THAT PURPOSE
Year: 1883

page_text: LETTERS PATENT to John Imray of N° 28 Southampton Buildings, Chaucery
Lane, in the county of Middlesex for an Invention of "IMPROVEMENTS IN The
PROCESS FOR EXTRACTING OILS BY DIFFUSION AND IN THE PREPARATION Of
MATERIALS AND ARRANGEMENT OF APPARATUS FOR THAT PURPOSE" com-
municated to him from abroad by Ivar Axel Bang and Charles Albert
Sanguinetti both of Paris in the Republic of France
PROVISIONAL SPECIFICATION left by the said John Imray at the Office
of the Commissioners of Patents on the 25th April 1883.
"
JOHN IMRAY of N° 28 Southampton Buildings Chancery Lane in the County of
Middlesex 'IMPROVEMENTS IN THE PROCESS FOR EXTRACTING OILS BY DIFFUSION
AND IN THE PREPARATION OF MATERIALS AND ARRANGEMENT OF APPARATUS FOR
THAT PURPOSE " [communicated to him from abroad by Ivar Axel Bang and
Charles Albert Sanguinetti both of Paris in the Republic of France]
According to this invention, a light and volatile hydrocarbon, obtained by
fractional distillation of petroleum, is purified by agitating it repeatedly with
sulphuric acid until colour disappears, and then has mingled with it a small
percentage of fuming or anhydrous sulphuric acid; this liquid decanted is employed
for extraction of oils in the following manner. A series of closed vessels, practically
about ten suffice, are arranged in order, the bottom of each communicating by a
pipe with the top of the next, and each having a tight fitting cover, an air cock,
and a glass gauge. The grains or fragments of vegetable matter or of bones, fat or
or other animal matter from which oil is to be extracted are enclosed in baskets
of wire net which are placed one in each of the vessels above mentioned. The first
vessel is charged with the hydrocarbon liquid which, after acting in it for about a
quarter of an hour, is transferred to the second vessel by forming a partial vacuum
in the latter, and the liquid thus passed from vessel to vessel acting in each case
by diffusion, that is to say, oil is extracted from the material in the baskets and
takes the place of part of the hydrocarbon which becomes absorbed by the material.

page_text: By the time the last vessel is reached, the liquid in it is pure oil, whilst the material
in the first vessel has all its oil extracted and contains hydrocarbon. The vessels
are arranged to act in rotation as above described, so that there is always at one
extreme of the range a vessel from which the oil is drawn, and at the other extreme
a basket of material from which the oil has been extracted, and which has to be
subjected to a farther operation for recovery of the hydrocarbon absorbed in it.
This is effected in the following manner. A small quantity of the hydrocarbon
liquid is vaporised, and its vapor is superheated by passing it through a heated
coil; this superheated vapor is admitted to act on the material and it has the effect
In
of vaporising all the contained hydrocarbon, which is condensed for future use.
some cases, it is of advantage to warm the diffusing vessels by hot water jackets,
or to warm the bydrocarbon which acts in them.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said John Imray in the Great Seal Patent Office on the 29th September
1883.
JOHN IMRAY of N° 28 Southampton Buildings Chancery Lane in the County of
Middlesex "
IMPROVEMENTS IN THE PROCESS FOR EXTRACTING OILS BY DIFFUSION
AND IN THE PREPARATION OF MATERIALS AND ARRANGEMENT OF APPARATUS FOR
THAT PURPOSE A communication to me from Abroad by Ivar Axel Bang and
Charles Albert Sanguinetti both of Paris in the Republic of France
"
Extraction of vegetable oils is usually effected by mechanical pressure with or
without heat, but 7 or 8 percent of oil is usually left in the cake. Attempts have
been made to avoid this loss by using solvents such as bisulphide of carbon, benzine,
essence of petroleum &c, but these attempts have been attended with difficulties
because these solvents have failed to produce a pure oil, and because the cake left
is utterly unfit to be used as food for animals. Thus the use of such solvents is
mostly confined to treatment of rancid matters or fats, in cases where the purity
of the products and by products is not important. Again, as good oil is damaged
by heating it above 80° or 90° Fahr., it is injured by the distillation necessary to
get rid of the solvents some of which it retains. Moreover, the residue is
impregnated with solvent which it is often very difficult to recover.
material treated be in pieces of some size, such as olives, fragments of bones and
the like, the volatile solvent can be expelled by steaming, but if crushed materials
be treated, the steam applied makes of the residue a cohesive paste from which the
solvent does not separate, and which is consequently of no commercial value.
If the
This invention has for its object to avoid the difficulties and evils attending the
extraction of oils as hitherto practised, by applying a diffusion process, that is to
say, subjecting the oleaginous materials to the action of a diffusing agent which
operates on them in the same way as in extraction of sugar by diffusion. As
diffusing agent a very volatile inodorous liquid is employed, such as leaves no trace
either in the product or in the residue. Chemically pure benzine may be used, or
light pure hydrocarbon obtained from petroleum and rendered inodorous by a
process hereinafter described, and this is applied by means of apparatus such as
illustrated by the accompanying drawings, Fig. 1 being an elevation of 3 of the
vessels constituting the battery, and Fig. 2 an elevation of the porous basket for
holding the material treated.
The process consists of the following steps of operation.
I. PURIFICATION OF THE DIFFUSING AGENT.
By preference the light hydrocarbon or essence distilled from petroleum is the
agent employed. It is first subjected to several fractional distillations until a very
volatile product is obtained boiling at 105° to 160° Fahr. Liquid of less volatility
might be used, but the more volatile is preferred in order to economise heat. The
product is several times agitated with sulphuric acid at 66° until the acid is not
discoloured, then about 2 or 3 per cent of fuming or anhydrous sulphuric acid is
added during violent agitation. The liquid thus obtained is very volatile and gives
1

page_text: for a time depending on the nature of the material treated, generally about a
quarter of an hour. The volatile liquid penetrates the material taking the place of
a portion of the oil which comes out of the material and mixes with the liquor in
the vessel. From the first vessel, which may be termed N° 1 of the battery, the
liquid is transferred to another of the same kind No 2. This is conveniently
effected by connecting the pipe S of No 2 to a vacuum chamber and opening the
cock of N° 1 and t of N° 2, these being connected by a pipe as shewn. The liquor
from N° 1, which is a mixture of the diffusing liquid with such oil as had been
extracted in N° 1, is allowed to act for about a quarter of an hour on fresh material
in N° 2, a fresh charge of diffusing liquid acting at the same time in N° 1. Thus
step-by-step the liquor is transferred through the series of vessels, of which there
should be about 10 in number, until finally there is left, little or no oil in the
material of N° 1, and pure oil exhausted of all the diffusing liquid in N° 10. '
III. RECOVERY OF THE DIFFUSING LIQUID.
The material in N° 1 vessel, being thoroughly impregnated with the diffusing
liquid, has to be treated for the recovery of the liquid for subsequent use, it being
first ascertained that no oil is left, by dropping a little of the liquor on paper, and
seeing that it entirely evaporates without leaving a trace of oil. First the cockr
is connected to a cooler and the liquid is allowed to run out into a receptacle.
When it ceases running, the cock is closed and 8 is connected to a pipe coil
immersed in a bath of hot liquid such as oil, glycerine or solution of chloride of
calcium. A little vapour of the diffusing liquid, obtained by boiling a portion, is
passed through this coil so as to become superheated to about 250° or 260° Fah*.
and admitted to the vessel R. The first portion of the vapour becomes condensed,
heating the saturated material in the vessel, and thereafter its heat vaporises the
imbibed liquid, and the vapour passes by the outlet T to a cooler where it is
condensed, and whence the recovered liquid flows to the receptacle. When it is
found that the temperature in the vessel R rises above the boiling point of the
liquid, the supply of vapour is stopped, and the vessel being opened the material is
taken out quite dry. In order to remove the last traces of diffusing liquid, a little
dry steam may be sent into the vessel before opening it.
The process above described is applicable not only to grains and other vegetable
oleaginous materials, but also to bones, fats and fishes. When materials contain
solid fats, the diffusing vessels should be slightly heated by hot water jackets, or
the diffusing liquid itself should be warmed.
Having thus described the nature of this invention and in what manner the
same is to be performed, as communicated to me by my foreign correspondents,
I claim -
First. The process, substantially as herein described, for extracting oils by
diffusion.
Second. For the purpose of extracting oils by diffusion, the use of volatile
hydrocarbon purified, substantially as herein described.
Third. The construction and arrangement of apparatus substantially as herein
described for extracting oils by the diffusive action of volatile bydrocarbon.
Fourth. The process, substantially as herein described, for recovering the
hydrocarbon from material treated for extraction of oil by diffusion..
In Witness whereof I the said John Imray have hereunto set my hand and
seal this Twenty ninth day of September in the year of our Lord One thousand
eight hundred and eighty-three.
JOHN IMRAV