Improvements relating to the Purification of Fatty Substances.
Year: 1891

page_text: Date of Application, 3rd June, 1891
Complete Specification Left. 22nd Feb., 1892-Accepted, 26th Mar., 1892
PROVISIONAL SPECIFICATION.
[Communicated from abroad by LA SOCIÉTÉ ANONYME DES PARFUMS NATURELS
DE CANNES, of 95, Boulevard Beaumarchais, Paris, in the Republic of
France.]
Improvements relating to the Purification of Fatty Substances.
1, 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:-
In former Specifications I have described two methods of purifying fatty
substances extracted by volatile solvents, based upon the use of steam and a
vacuum under certain conditions. Although either of these two methods attains
the object aimed at, that is to say the complete elimination of the last traces of the
solvent in fatty substances subjected to the treatment, both have the defect of
causing condensation of water in the interior of the fatty mass. Now it is well
known how small a quantity of water is sufficient to give a dim appearance to the
best oils thus depreciating their value, and it is also known how difficult it is to
eliminate these last traces of water when thus contained in a fatty substance.
When the aforesaid two methods are employed considerable emulsion of water
and fatty substance takes place enclosing small quantities of the solvent the
inconveniences of which it is easy to understand.
Now the present invention relates to a method which remedies these imperfections
and gives at once limpid or unclouded oils without further treatment and without
loss of the fatty substance or of the solvent.
As in the above mentioned methods recourse is had to the simultaneous action of
steam and a vacuum but under conditions which prevent all condensation of water
in the interior of the fatty mass while at the same time causing the vapours of the
solvent to be carried away by an energetic dashing and stirring movement.
When the evaporation of the solution is effected in a vacuum there will be a
moment when there is no ebullition of the solvent, although the material still
contains a considerable proportion thereof.
This moment it is easy to recognize first by observing the material under operation
the apparatus being provided with glass windows, and also if the heating continues
by the rise of temperature while the vacuum augments. At this moment the
improved method of purification is used for completely driving out the last traces
of the solvent without introducing water into the fatty substance.
At the said moment the temperature of the fatty substance to be purified in the
apparatus, is raised to a higher degree than the boiling point of the water for the
vacuum existing in this apparatus, and into the mass steam as thoroughly dried as
possible is introduced by one or more jets, the said steam being at a slight pressure.
For this purpose use can be made of exhaust steam from steam engines. It is
however useful that this jet or these jets shall be disposed so as to cause in the
fatty mass a sufficiently energetic agitation for continually bringing fresh parts of
this mass in contact with the steam and prevent any particle escaping from the
action of the latter. The employment of injectors enables this result to be
obtained in a very simple manner.
The steam thus introduced into the apparatus will not condense and the few
drops of water which it may contain will be vaporized by the heat of the fatty
material. In fact during the operation the mass is constantly kept at a higher
temperature than that corresponding to the boiling point of the water this degree
of vacuum by heating it through the medium of a serpentine or double bottom in

page_text: which steam circulates. This heating is needful because without it the mass
would be cooled in the first place by the volatilization of the solvent and in the
second place by the evaporation of the drops of water always carried away by the
steam whatever care may be taken for getting rid of the same prior to the passage
into the apparatus which drops are also caused by the expansion of the steam from
the pressure at the introduction to the vacuum existing in the apparatus.
It should be observed that the temperature at which the fatty substance is liable
to undergo a change must never be excecded in the fatty mass contained in the
apparatus.
This temperature being determined regulates in its turn the temperature of the
steam which must also be in the apparatus some degrees lower than that of the
fatty mass.
The temperature of the steam determines the degree of vacuum at which the
operation is to take place by virtue of the relations existing between the boiling
point of any liquid and the pressure to which it is subjected.
The above mentioned difference of temperature between the fatty body and the
steam in the interior of the apparatus must be the higher and the vacuum the
greater the higher the boiling point of the solvent: this difference must also be
the greater the less dry the steam.
It will be expedient if the fatty substance is susceptible of changing at a lower
temperature than 100 degrees centigrade to expand also the steam entering the
double bottom by producing in the latter a sufficient vacuum to make sure that in
no case the temperature of the heated part of this double bottom shall reach the
degree at which the fatty substance might undergo a change. Under these
conditions the steam acts upon the fatty substance in the apparatus similarly to a
gas, but of a gas which is afterwards condensed in the condenser at the same time
as the vapours of the solvent and does not interfere at all with the condensation of
the latter so that the last traces of the same can be collected and loss obviated.
Dated this 3rd day of June 1891.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements relating to the Purification of Fatty Substances.
1, 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 :-
In former Specifications No. 10280 of 1889 and No. 5940 of 1890 I have
described two methods of purifying fatty substances extracted by volatile solvents,
based upon the use of steam and a vacuum under certain conditions.
Although either of these two methods attains the desired object that is to say,
the complete elimination of the last traces of the solvent in fatty substances
subjected to the treatment, both have the defect of causing condensation of water
in the interior of the fatty mass. Now it is well known how small a quantity of
water is sufficient to give a dim appearance to the best oils thus depreciating their
value and it is also known how difficult it is to eliminate these small quantities of
water when thus contained in a fatty substance.
When the aforesaid two methods are employed considerable emulsions of water
and fatty substance takes place enclosing small quantities of the solvent the
inconveniences of which it is easy to understand.
Now the present invention relates to a method by which the above mentioned
imperfections are overcome and which gives at once limpid or unclouded oils
without further treatment and without loss of the fatty substance or of the solvent.

page_text: As in the above-mentioned methods recourse is had to the simultaneous action
of steam and a vacuum, but under conditions which prevent all condensation of
water in the interior of the fatty mass while at the same time causing the vapours:
of the solvent to be carried away by an energetic dashing and stirring movement.
When the evaporation of the solution is effected in a vacuum there will be a
moment when there is no ebullition of the solvent, although the material still
contains a considerable proportion thereof.
:
This moment it is easy to recognise, first by observing the material under
operation, the apparatus being provided with glass windows, and also if the heating
continues, by the rise of temperature while the vacuum augments. At this moment.
the improved method of purifications is used for completely driving out the last
traces of the solvent without introducing water into the fatty substance.
At the said moment the temperature of the fatty substance to be purified in the
apparatus, is raised to a higher degree than the boiling point of the water for the
vacuumn existing in this apparatus and into the mass, steam as thoroughly dried as
possible is introduced by one or more jets, the said steam being at a slight pressure.
For this purpose use can be made of exhaust steam from steam engines. It is
however useful to so arrange this jet or these jets as to cause in the fatty mass, a
sufficiently energetic agitation for continually bringing fresh parts of this mass in
contact with the steam and prevent any particle escaping from the action of the
latter. The employment of injectors enables this result to be obtained in a very
simple manner.
The steam thus introduced into the apparatus will not condense and the few
drops of water which it may contain will be vaporized by the heat of the fatty
material. In fact during the operation the mass is constantly kept at a higher
temperature than that corresponding to the boiling point of the water under this
degree of vacuum, by heating it through the medium of a serpentine or double
bottom in which steam circulates. This heating is necessary because without it
the mass would be cooled in the first place by the volatilization of the solvent and
in the second place by the evaporation of the drops of water always carried away
by the steam whatever care may be taken for getting rid of the same prior to the
passage into the apparatus, which drops are also caused by the expansion of
the steam from the pressure at the introduction to the vacuum existing in the
apparatus.
It should be observed that the temperature at which the fatty substance is
liable to undergo a change must never be exceeded in the fatty mass contained in
the apparatus.
This temperature being determined regulates in its turn the temperature of the
steam which must also be, in the apparatus, some degrees lower than that of the
fatty mass.
The temperature of the steam determines the degree of vacuum at which the
operation is to take place by virtue of the relations existing between the boiling
point of any liquid and the pressure to which it is subjected.
The above mentioned difference of temperature between the fatty body and the
steam in the interior of the apparatus must be the higher and the vacuum the
greater, the higher the boiling point of the solvent, this difference must also be
greater the more moisture is contained in the steam.
It will be expedient if the fatty substance is susceptible of changing at a lower
temperature than 100 degrees centigrade to expand also the steam entering the
double bottom by producing in the latter a sufficient vacuum to make sure that in
no case the temperature of the heated part of this double bottom shall reach the
degree at which the fatty substance might undergo a change. Under these
conditions the steam acts upon the fatiy substance in the apparatus similarly to a
gas, but of a gas which is afterwards condensed in the condenser at the same time
as the vapours of the solvent, and does not interfere at all with the condensation of
the latter, so that the last traces of the same can be collected and loss obviated.

page_text: 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 method of purifying fatty substances extracted by volatile
solvents, based upon the simultaneous employment of a vacuum and dry steam at
a low pressure projected in the form of a jet into the midst of the fatty material,
this material being maintained at a temperature which prevents the steam from
condensing under the conditions in which the operation takes place, as hereinbefore
described.
Dated this 22nd day of February 1809
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.