Improvements relating to the Purification of the Residues or Cakes Obtained from Fatty Substances, Oleaginous Fruits, or Grains.
Year: 1891

page_text: The decision of the Comptroller-General, of the 31st day of October 1894
allowed, under Section 18 of the Patents, &c. Act, 1883, an Amendment of
this Specification.
Date of Application, 29th Sept., 1891
Complete Specification Left, 20th June, 1892-Accepted, 23rd July, 1892
PROVISIONAL SPECIFICATION.
DES PARFUMS
NATURELS DE CANNES, of 95, Boulevard Beaumarchais, Paris, in the
Republic of France.]
Improvements relating to the Purification of the Residues or Cakes
Obtained from Fatty Substances, Oleaginous Fruits, or Grains.
[Communicated from abroad by LA SOCIÉTÉ ANONYME
I, HENRY HARris Lake of the Firm of Haseltine Lake & Co., Patent Agents,
45 Southampton Buildings, in the County of Middlesex, do hereby declare the
nature of this invention to be as follows:--
This invention relates to the purification of the residues or cakes obtained from
fatty substances, oleaginous fruits or grains.
One of the chief obstacles which has hitherto opposed the greater extension of
processes of extraction by volatile solvents in the manufacture of oils and fats
arises from the fact that it is difficult and in certain cases almost impossible by the
well-known methods to free the exhausted material from the solvent which it retains
after the oil has been withdrawn without destroying its qualities as manure or
alimentary cake or without losing too great a quantity of the said solvent.
On the one hand the use of hot air or other gas, even if it has the advantage of
not changing the nature of the residue causes a certain amount of loss of the
solvent which largely augments the cost price of the said solvent; on the other
hand it has been found that the employment of steam under conditions heretofore
practised is applicable only to a limited number of cases.
If for example amylaceous materials are treated the water condensed causes the
whole mass to form a paste which promptly arrests all ulterior action so that there
is at the same time a change in the material treated and an increased loss of
solvent. Moreover, even in cases where the operation itself may be considered
successful the cake requires to be dried, which further increases the cost of
manufacture.
The improved method hereinafter described has for its object to obviate the
inconveniences above referred to and to enable dry cakes to be obtained from all
oleaginous fruits and grains without the odour of the solvent and possessing
all their useful qualities. It is also based upon the results obtained by the method,
in respect of which an application for Letters Patent, No. 9431, was filed on the
3rd of June 1891, under the title of "Improvements relating to the purification of
fatty substances use being made of the aforesaid method in the case of more or
less pulverulent solid substances.
Accordingly for freeing the exhausted material (residue or cake) from the solvent
which it retains steam is employed with or without a vacuum but under conditions
which prevent all condensation in the material treated. The steam carries away
to the condenser the last traces of the solvent after the manner of a gas, but of a

page_text: gas which can be condensed at the same time as the vapour of the solvent with
which it is mixed to such an extent that the whole is collected in the liquid state
without any loss.
The condensation of the steam in the midst of the material under treatment is
avoided by subjecting this material to a temperature above the boiling point of the
water for the pressure at which the treatment is effected. In the method respecting
which the above-mentioned application for Letters Patent No. 9431 was filed this
result is obtained by heating the fatty substance in the liquid state by means of a
double bottom wherein steam circulates; in the present instance on account of the
more or less pulverulent state of the material, this method would be impracticable
and unsuccessful. This difficulty is overcome by communicating beforehand to the
material a sufficient excess of heat through the medium of a current of steam,
superheated at a suitable temperature, the mode of operation being as follows:-
When the material has been exhausted, and while it is still in the extractor,
vapour from the superheated solvent is introduced from the top of this extractor
the liquid solvent retained in the material is displaced little by little, and even
distilled, the temperature in the extractor gradually rising to the boiling point of
the solvent. Instead of now stopping the introduction of the vapour from the
solvent as heretofore practised by those who also employ vapour from the super-
heated solvent, the introduction of this vapour is continued until the entire mass in
the extractor has obtained the desired temperature.
At this moment a current of dry steam is introduced through the top of the
extractor, and owing to the excess of heat previously communicated to the material
the steam does not condense but being lighter than the vapour from the solvent it
displaces the latter.
The cake is then freed from all odour of the solvent and contains only a very
small amount of moisture.
It is expedient to superheat the steam before its introduction into the extractor
so as to overcome the cooling and to maintain the material under treatment more
easily at the proper temperature, which should as before said be above the boiling
point of the water for the pressure at which the operation takes place. The degree
to which this steam can thus be superheated depends on the temperature from which
the material under treatment is susceptible of change under existing conditions.
If the material operated upon is susceptible of change at about 100 degrees
centigrade it is advisable to produce a partial vacuum in the apparatus prior to the
introduction of steam so that the boiling point of the water at this pressure shall be
lower by some degrees than the temperature at which the mass is susceptible of change.
Dated this 29th day of September 1891.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.
COMPLETE SPECIFICATION (AMENDED).
Improvements relating to the Purification of the Residues or Cakes
Obtained from Fatty Substances, Oleaginous Fruits, or Grains.
I, HENRY HARRIS LAKE, of the Firm of Haseltine Lake & Co., Patent Agents,
45 Southampton Buildings, in the County of Middlesex, do hereby declare the
nature of this invention and in what manner the same is to be performed to be
particularly described and ascertained in and by the following statement:-
This invention relates to the purification of the residues or cakes obtained from
fatty substances, oleaginous fruits or grains.
One of the chief obstacles which has hitherto opposed the greater extension of
processes of extraction by volatile solvents in the manufacture of oils and fats
arises from the fact that it is difficult and in certain cases almost impossible by the

page_text: well-known methods to free the exhausted material from the solvent which it retains
after the oil has been withdrawn without destroying its qualities as manure or
alimentary cake or without losing too great a quantity of the said solvent.
On the one hand the use of hot air or other gas even if it has the advantage of
not changing the nature of the residue causes a certain amount of the solvent
which largely augments the cost price of the said solvent on the other hand it has.
been found that the employment of steam under conditions heretofore practised is
applicable only to a limited number of cases.
If for example amylaceous materials are treated the water condensed causes the
whole mass to form a paste which promptly arrests all ulterior action so that there
is at the same time a change in the material treated and an increased loss of solvent.
Moreover, even in cases where the operation itself may be considered successful
the cake requires to be dried, which further increases the cost of manufacture.
The improved method hereinafter described has for its object to obviate the incon-
veniences above referred to and to enable dry cakes to be obtained from all oleaginous
fruits and grains without the odour of the solvent and possessing all their useful
qualities. It is also based upon the results obtained by the method in respect of
which an application for Letters Patent No. 9431 was filed on the 3rd June 1891
under the title of "Improvements relating to the purification of fatty substances,"
use being made of the aforesaid method in the case of more or less pulverulent
solid substances.
Accordingly for freeing the exhausted material (residue or cake) from the
solvent which it retains steam is employed with or without a vacuum but
under conditions which prevent all condensation in the material treated. The
steam carries away to the condenser the last traces of the solvent after the manner
of a gas but of a gas which can be condensed at the same time as the vapour of
the solvent with which it is mixed to such an extent that the whole is collected in
the liquid state without any loss.
The condensation of the steam in the midst of the material under treatment is
avoided by subjecting this material to a temperature above the boiling point of the
water for the pressure at which the treatment is effected. In the method respecting
which the above-mentioned application for Letters Patent No. 9431 was filed this
result is attained by heating the fatty substances in the liquid state by means of a
double bottom wherein steam circulates; in the present instance on account of the
more or less pulverulent state of the material, this method would be impracticable
and unsuccessful. This difficulty is overcome by communicating beforehand to the
material a sufficient excess of heat through the medium of a current of steam,
superheated at a suitable temperature, the mode of operation being as follows:
When the material has been exhausted, and while it is still in the extractor
vapour from the superheated solvent is introduced from the top of this extractor the
liquid solvent retained in the material is displaced little by little, and even distilled,
the temperature in the extractor gradually rising to the boiling point of the solvent.
Instead of now stopping the introduction of the vapour from the solvent as
heretofore practised by those who also employ vapour from the superheated solvent
the introduction of this vapour is continued until the entire mass in the extractor
has obtained the desired temperature.
At this moment a current of dry steam is introduced through the top of the
extractor and owing to the excess of heat previously communicated to the material
the steam does not condense but being lighter than the vapour from the solvent it
displaces the latter.
The cake is then freed from all odour of the solvent and contains only a very
small amount of moisture.
It is expedient to superheat the steam before its introduction into the extractor
so as to overcome the cooling and to maintain the material under treatment more
easily at the proper temperature which should as before said be above the
boiling point of the water for the pressure at which the operation takes place.
The degree to which this steam can thus be superheated depends on the temperature

page_text: from which the material under treatment is susceptible of change under existing
conditions.
If the material operated upon is susceptible of change at about 100 degrees
centigrade it is advisable to produce a partial vacuum in the apparatus prior to the
introduction of steam so that the boiling point of the water at this pressure shall
be lower by some degrees than the temperature at which the mass is susceptible of
change.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, as communicated to me by
my foreign correspondents, I declare that what I claim is :-
The improved process for purifying the residues or cakes obtained from fatty
matter oleaginous fruit or grain, treated by volatile solvents, (constituting an
application of the method described in the Specification of Letters Patent
No. 9431 of 1891 to more or less pulverulent solid matter) which is based upon the
use of any steam under conditions preventing the condensation of water in the
exhausted material and which results in a residuum or dry cake free from the smell
of the solvent and unaltered substantially as above described employment firstly of a
current of superheated vapour of the solvent, and secondly of a current of dry steam,
substantially as, and for the purposes, specified, whereby a residuum or dry cake free
from the odour of the solvent, and unaltered, is obtained.
Dated this 20th day of June 1892.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.