A NEW OR IMPROVED PROCESS FOR THE INTEGRAL EXTRACTION OF THE CONSTITUENT PRINCIPLES OF FATTY BODIES
Year: 1882

page_text: LETTERS PATENT to William Henry Beck of 139 Cannon Street in the City
"
of London Consulting Engineer and Patent Agent for an Invention of
A NEW OR IMPROVED PROCESS FOR THE INTEGRAL EXTRACTION OF THE
CONSTITUENT PRINCIPLES OF FATTY BODIES Communicated to him from
abroad by Charles Violette and Alphonse Buisine both of Lille in the Republic
of France
PROVISIONAL SPECIFICATION left by the said William Henry Beck at
the Office of the Commissioners of Patents on the 4th October 1882.
WILLIAM HENRY BECK of 139 Cannon Street in the City of London, Consulting
Engineer and Patent Agent, "A NEW OR IMPROVED PROCESS FOR THE INTEGRAI.
EXTRACTION OF THE CONSTITUENT PRINCIPLES OF FATTY, BODIES "[Commuicated
to him from abroad by Charles Violette and Alphonse Buisine both of Lille in the
Republic of France]
The process forming the subject of the present invention allows of the integral
extraction of the constituent principles of fatty bodies, that is to say, the glycerine.
and solid and liquid fatty acids which enter into their composition, and that too
without injury to any of them-The fatty bodies, tallows, greases or oils liquified
in a reservoir are introduced along with a suitable proportion of commercial
ammonia into a metallic digester enamelled on the inside-For one hundred
kilo-grammes of fatty matter there are required theoretically five kilo-grammes, two
hundred and fifty grammes of pure ammoniacal gas (Az H³) say about thirty litres
of commercial ammonia at twenty-two degrees Baumné, with five litres of water
added.
The digester is furnished with an outlet tube, a pipe for the entrance of steam or
compressed air, an air pipe in communication with a condensing column, a pressure
gauge, a safety valve and a cock for taking out samples. It is heated directly by
the flame from a furnace which flame circulates round the apparatus in suitably

page_text: constructed flues. A damper adapted to close the opening to the said flues entirely
if desired allows of regulating the temperature of the digester at pleasure. When
the damper is closed the flame is sent into another flue and utilized for heating a
second digester or otherwise. The temperature is raised progressively so as to
maintain the pressure during several hours between five and seven atmospheres,
more or less, the raising of the pressure shortening the duration of the reaction.
The ammoniacal saponification being effected, a. communication is opened
between the digester and a boiler by suitable cocks, and immediately the pressure
which exists in the digester forces the liquid matter through the outlet tube into
the said boiler. The whole mass is forced out if required by introducing high
pressure steam or compressed air into the digester through the steam or compressed
air pipe.
The boiler, which is heated by a superheated steam coil and by the waste heat
from the aforesaid furnace, communicates by its neck with a coil and condensing
column. The dissociation of the ammoniacal soap commences as soon as it arrives
into the aforesaid boiler, and is completed by heating the mass by the help of the coil
therein, and by progressively raising the temperature to one hundred and eighty
degrees Centigrade. In a few hours the decomposition is complete. The aqueous
vapour disengaged at the same time as the ammonia is condensed in the condensing
coil, and the ammonical liquid runs from the reservoir at the bottom thereof
through a cock into a suitable receptacle-This aminoniacal water is utilized again
in the following operations. The uncondensed ammoniacal gas passes by a suitable
passage into the condensing column where it is entirely absorbed by water which
falls from the upper part of the said column. The ammoniacal solution is collected
to serve in the subsequent operations. In the meantime the digester is recharged
when suitably cooled-Tho mixture of glycerine and fatty acids, absolutely pure
and uninjured, is taken from the boiler to a reservoir containing water heated by a
perforated steam pipe, and is there submitted to an energetic beating by an
agitator. The aqueous liquid flows away through a cock, and, after several
washings, the fatty acids freed from glycerine, are conveyed through another cock
to a special reservoir. The fatty acids suitably cooled, are submitted to pressure
and separated into solid fatty acids, which, after filtration or distillation if
necessary, are fit for the manufacture of candles, and into oleic acid of saponification,
which does not contain any product of decomposition and is eminently suitable for
the industrial uses to which that fatty acid is applicable. The aqueous liquid being
slightly milky, a small quantity of sulphuric or hydrochloric acid is added which
removes that appearance. By decantation the aqueous part which contains all the
glycerine is separated and at the same time a certain quantity of the fatty acids,
soluble in water, such as buteric (butyrique) valeric (valérique) and so forth. By
treating the liquid with lime or an analogous base, the slightly soluble buterates
(butymtes) valerates (valérates) and so forth of lime are to a great extent
precipitated, these may be utilized for extracting from them the buteric, valeric and
other acids, afterwards the glycerine is extracted from its aqueous solution. and
then purified by the ordinary processes.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said William Henry Beck in the Great Seal Patent Office on. the
2nd April 1883.
WILLIAM HENRY BECK; of 139 Cannon Street, in the City of London, Consulting
Engineer and Patent Agent "A NEW OR IMPROVED PROCESS FOR THE INTEGRAL
EXTRACTION OF THE CONSTITUENT PRINCIPLES OF FATTY BODIES" [Communi-
cated to him from abroad by Charles Violette and Alphonse Buisine, both of
Lille in the Republic of France]
The process forming the subject of the present invention consists in heating the
fatty body, such as oil, tallow or grease, under pressure, with an aqueous solution
of Ammonia. Under these circumstances an ammoniacal soap is formed, and the
glycerine is set free. This ammoniacal soap, being removed from the digester, is
heated in the open air, and is completely decomposed into ammonia, which is
collected, and into free fatty acids. The glycerine, liberated in the first operation,
is found mixed with these fatty acids, and a simple washing in water separates it..
Thus there are obtained, on the one hand; pure uninjured fatty acids, and on the
other hand, glycerine in an aqueous solution; the ammonia serves as inter-
mediary only in the operation, and may be used again and again indefinitely.
The drawing hereto annexed represents a demonstrative section of an apparatus
suitable for the process.
The fatty bodies, such as tallows, greases or oils, liquified in a reservoir A, are
introduced, along with a suitable proportion of commercial aminonia, from the
reservoir G, through the tube B, into a metallic digester C, which may be of cast
or wrought iron or copper enamelled or tinned on the inside, or lined with sheet
lead. The two-liquids may be introduced into the digester either separately.or
sinultaneously. For 100 kilogrammes of fatty matter there are required
theoretically 5 kilogrammes 250 grammes of pure ammoniacal gas (Az. H³), say
about, 30 litres of commercial ammonia at 22° Baumé, with 5 litres of water
added.
The digester C is furnished with an outlet tube D, a pipe F for the entrance, as
may be required, of steam or compressed air, an air pipe E in communication with
a condensing column T, a pressure gauge m, safety valves and a cock for taking
out samples. It is either heated directly by the flame from a furnace (not shown),
which flame circulates round, the apparatus in suitably constructed flues K, or by
the circulation of water or steam in the tubes h, one of which is shown more clearly
in a detached figure at H, or by both systems combined. When the beating is
effected by the circulation of steam or hot water, the steam or water is introduced
by the pipe H', and after giving up its heat, by its passage through the tubes h, it
returns to the boiler by the pipe I. The temperature is raised progressively so as
to maintain the pressure during several hours between 5 and 7 atmospheres, more
or less, the raising of the pressure shortening the duration of the reaction.
Samples taken from time to time enable the progress of the operation to be
judged of.
The ammoniacal saponification being effected, the cocks L, E and F. remaining
closed, the valve L' is opened, and immediately the pressure which exists in the
digester forces the liquid matter, through the outlet tube D D, into a tank J, (the
upper part of which communicates by a pipe F¹ with the condensing column T) and
from thence, by the pipe J¹, into the boiler M.
The boiler M, which is heated by a superheated steam coil N, and by the waste
heat from the aforesaid furnace K, communicates, by its neck O, with a coil P and
the condensing column T. The dissociation of the ammoniacal soap commences as
soon as it reaches the aforesaid boiler M; and is completed by heating the mass,
by the help of the coil N therein, by progressively raising the temperature to about

page_text: 180° Centigrade, and by blowing in a little air by the second coil N'. 'In a few
hours the decomposition is complete. The aqueous vapour disengaged at the saine
time as the ammonia, is condensed in the condensing coil P, and the ammoniacal
liquid runs from the reservoir at the bottom thereof, through a cock R, into a
suitable receptacle. This ammoniacal water is utilized again in the following
operations. The uncondensed ammoniacal gas passes, by a suitable passage S, into
the condensing column T, where it is entirely absorbed by water which falls from
the upper part U of the said column. The ammoniacal solution is collected at V to
serve in the subsequent operations. In the meantime the digester C is recharged
when suitably cooled, and in order to avoid loss of animonia while charging, the
pipe E is put into communication with the lower part of the column T. The
mixture of glycerine and fatty acids, entirely pure and uninjured, is taken from the
boiler M to a reservoir X containing water heated by the perforated steam pipe Z,
and is there submitted to an energetic beating by an agitator Y. The aqueous
liquid flows away through a cock W, and, after several washings, the fatty acids
freed from glycerine, are conveyed through another cock W to a special reservoir.
The last traces of ammonia may be removed more quickly by adding a small
quantity of sulphuric acid to the washing water. The fatty acids; cooled in any
suitable way, are submitted to pressure and, separated into solid fatty acids, which,
after filtration or distillation if necessary, are fit for the manufacture of candles,
and into oleic acid of saponification, which does not contain any product of decom-
position and is eminently suitable for the industrial uses to which that fatty acid
is applicable. The aqueous liquid being elightly milky, a very small quantity of
sulphuric or bydrochloric acid is added which removes that appearance. By
decantation, the aqueous part, which contains all the glycerine, is separated, and
at the same time a certain quantity of the fatty acids, soluble in water, such as
buteric, (butyrique) valeric, (valérique) and so forth. By treating the liquid with
lime or an analagous base, the slightly soluble buterates (butyrates), valerates
(valérates), and so forth of lime are to a great extent precipitated; these may be
utilized for extracting from them the buteric, valeric, and other acids; afterwards
the glycerine is extracted from its aqueous solution, and then purified by the
ordinary processes.
After saponification, the ammoniacal soap can also be decomposed by hydro-
chloric and sulphuric acids: by beating in water, glycerine, hydrochlorate or
sulphate of ammonia in solution, and fatty acids soluble in water are obtained.
The aqueous liquor boiled with lime yields ammonia; the precipitato yields the
buterates and valerates of lime; and the glycerine can be withdrawn from the
liquid by the ordinary processes. The fatty acids are separated into solids and
liquids by pressure.
In some special cases the ammoniacal soap can be treated with chlorine or
calcium; and the precipitated calcareous soap thus obtained, and in a very divided
state, is easily decomposed by mineral acids.
It is not absolutely indispensable to use the theoretic quantity of ammonia
necessary for transforming all the fatty acids of oils and greases into ammoniacal
sonp as just described, as the decomposition of fatty bodies into their constituent
principles can be effected equally well, in this apparatus, with a quantity of
ammonia much below that indicated by theory; for example, with one third or a
quarter of the quantity, and even with a much smaller fraction, but in the latter
case it would require much inore time to effect the complete reaction. For these
'new conditions of ammoniacal saponification, with simultaneous dissociation of the
soap formed in the digester, the following mode of operation appears to be the
best: the liquid fatty body is introduced into the digester C, as already described
fabove, with the aminoniacal solution, in such manner that for 100 kilogrammes of
the fatty body 10 litres of ammonia of commerce at 22° Baumé, and 25 litres of
water are used, that is, one third of the theoretical quantity of ammonia.
The digester is heated by fire applied direct, or by circulation of steam or hot
water, and a pressure of from 5 to 7 atmospheres, more or less, is maintained for

page_text: some hours. When the reaction is finished, the cocks L, E, and F being closed, the
valve L' is opened, and the pressure in the apparatus forces the líquid through the
pipe into an appropriate reservoir. The apparatus is completely emptied, when
required, either by steam or by compressed air introduced through the pipe F.
After standing a sufficient time, the liquid mass separates into two layers; the
lower aqueous part, containing the whole of the water, is decanted, and may be
added to the ammonia at 22° used in the next operation, or it may be treated for
the recovery of the small quantity of ammonia, glycerine, and the buteric and
valeric acids that it contains. The oily part, mixed with free fatty acids,
ammoniacal soap, these same fatty acids dissolved, and glycerine, is sent into the
boiler M; the operation is then finished in the manner already described above.
By applying this process to oils and greases not very rich in solid fatty acids,
the separation of the solid fatty acids from the oleic need not be effected, and
there is then obtained from all the oils, even the most refractory to ordinary
saponification, a mixture of fatty acids, deprived or not of glycerine, which is
immediately saponifiable and capable of furnishing, without difficulty, soaps with
potash and soda bases. If it is desired to obtain either calcareous or insoluble
soaps from other bases, the addition of ammonia in the digester facilitates their
production. Either lime and a small quantity of ammonia, or chloride, of calcium,
or any other earthy or metallic chloride and ammonia, in quantities equivalent
and sufficient to form an insoluble soap, is added to the fatty body. The digester
is maintained at between 5 and 7 atmospheres of pressure. The ammoniacal soap
as it forms furnishes, by double decomposition, a soap which is precipitated, and in
the case of ammonia and lime, the ammonia is reproduced at every moment.
When the chlorides and ammonia are used the latter is recovered in the aqueous
liquid in the form of hydrochlorate of ammonia, from which the ammonia may be
extracted by distillation with lime and glycerine by the ordinary processes.
This saponification, which may be called ammonio-calcareous or ammonio-metallic,
shortens the operation very much, and this decomposition of the fatty body may
be effected at a lower pressure than when line alone is used.
Having now described the nature of the said Invention and the manner in
which the same is to, or may be carried into effect, I would have understood.
that what I claim as. the invention to be secured by the within in part recited
letters patent is :-
First. The application of the ammoniacal saponification effected under pressure, and
of the decomposition of ammoniacal soap by dissociation by heat and at the
ordinary pressure substantially as hereinbefore described for the purpose of
depositing from the fatty bodies the glycerine and the fatty acids they contain,
the ammonia in the process acting only as an intermediate agent which may
be used over and over again indefinitely.
Second. The saponification of fatty bodies hereinbefore called ammonio-calcareous,
or ammonio-metallic saponification, with recovery of the ammonia, substan-
tially as herein before described.
Third. The general arrangement and combination of apparatus hereinbefore
described, and illustrated in the drawings, and for the purpose of carrying
out the processes hereinbefore described.
In witness whereof I, the said William Henry Beck have hereunto set my
hand and seal this Thirty-first day of March in the year of our Lord One
thousand eight hundred and eighty.three