Improvements in Processes for Producing Chemical Combinations from Raw Wool Fat.
Year: 1896

page_text: Date of Application, 6th Aug., 1896-Accepted, 21st Nov., 1896
COMPLETE SPECIFICATION.
Improvements in Processes for Producing Chemical Combinations
from Raw Wool Fat.
I, CARL SCHMIDT, of Magdeburg Buckau, in the Empire of Germany, Doctor
of Philology, 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 producing by steps acid wool fat free of sebacic acids,
sebacic acids, combinations with a high melting point fit for the manufacture of
candles, and fatty alcohols of raw wool fat whereby by clarifying the fat alcohols
combinations of the latter with water are produced possessing wax of a salve like
consistency and which I call lanoglycerine."
It is known that raw wool fat consists essentially of ether like combinations
of higher and lower sebacic acids with cholesterine, isocholesterine, and fat
alcohols. It contains besides free sebacic acids mostly fat alcohols and
cholesterine.
The present process is divided into four steps, the succession of which can be
changed in any manner, by which is produced firstly, a separation into one part
consisting of the raw wool fat containing nearly exclusively sebacic acids and then
into another part consisting of a combination of sebacic acids and fat alcohols,
whereby as an intermediary product neutral wool fat can be obtained.
From these combinations of sebacic acids and fat alcohols by appropriate treat-
ment combinations can be obtained melting between 60-75° C. which consist
essentially of sebacic acids the remaining portion being divided into nearly pure
sebacic acids and fat alcohols which latter still contain a few sebacic acids.
Finally a product 1 call lanoglycerine is obtained by treating the fat alcohols
with water.
Under the term fat alcohols is understood the mixture of cholesterine
isocholesterine and the other fat alcohols contained in wool fat.
In order to separate the raw wool fat into nearly pure sebacic acids on one side
and into a combination of sebacic acids and fat alcohols on the other side one
proceeds in the following manner.
1. If wool fat is treated conveniently at water bath temperature with a double
quantity of alcoholic ammonia, 20-30% of the fat is easily dissolved, the free
sebacic acids being converted into ammonia salts and a part of the wool fat being
divided into sebacic acid amides and free fat alcohols.
If after depositing, the still warm alcoholic solution is decanted from the deposit
and the latter is boiled several times with alcohol, a completely neutral wool fat
remains.
A complete decomposition of the wool fats by means of alcoholic ammonia can
only be obtained by repeating several times the described operation with the deposit
until the complete solution of the wool fat is obtained or by introducing ammonia
gas into a boiling mixture of alcohol and wool fat until complete solution is
obtained.
As however the reaction after the decomposition and the solution of about 50% of
the wool fat operates slowly, it is preferable to obtain the effect under pressure by
applying pressure at once from the beginning or after decomposition of 20-30%
of the wool fat.
.

page_text: For this purpose the wool fat is placed in a closed apparatus which may be fitted
with an agitator, and with gradual increase of temperature it is heated with the
requisite quantity of alcoholic ammonia until all the wool fat is dissolved and it is
left under pressure until it is found by treating a sample drawn from the reaction
product that after it has cooled it will become fluid and dissolve again on warming
under ordinary atmospheric pressure.
In all cases alcoholic solutions are obtained which by cooling deposit
crystalline combinations a mixture of fat alcohols and ammonia fat acid
combinations whilst nearly pure sebacic acids remain dissolved. The solid.
combinations are separated in a convenient manner from the alcoholic solution the
latter is freed by distillation from alcohol and ammonia and the deposit is heated.
with acids until the sebacic acids are parted with which are then worked further in
the known manner.
The solid combinations are freed in the same manner from alcohol and ammonia
and treated with acids. The resulting product representing the said mixture of
fat alcohols and sebacic acids.
2. When saponified wool fat-which can be produced in the known manner for
instance by means of alcoholic alkalies and decomposition of the reaction product
with acids or by distillation with or without superheated steam and in or without
a vacuum or in any other manner-is treated with alcoholic ammonia it is
completely dissolved. By cooling, a mixture of fat alcohols and sebacic acid
ammonia salts is parted with whilst nearly pure sebacic acids remain dissolved.
The combinations are separated as before and can be further worked.
The used alcoholic ammonia can be produced either from diluted or from
absolute alcohol for instance by introducing ammonia gas or by mixing alcohol
with watery ammonia.
By using strongly diluted. alcoholic ammonia only sebacic acids are dissolved.
whilst the mixture of the fat alcobols and of the other sebacic acids is obtained
as a deposit.
3. This separation can also be obtained by the distillation of the raw wool fat in
fractions with or without a vacuum or with superheated steam by receiving the
first oily distillate amounting to 50% of the wool fat separately from the later
product of half solid consistence and by separating the latter again by distillation
in an oily and in a more solid product. This latter more solid product represents
equally a wool fat saponified and freed from a part of its sebacic acids.
When at the water bath temperature such a saponified wool fat freed from a
part of its sebacic acids is dissolved in acetone, there are deposited by cooling solid
crystalline combinations, which are filtered and washed with acetone until they.
look nearly pure white. The satne after being freed from acetone and dried
at 100° C. constitute an oil, which on cooling congeals to a crystalline mass, which
according to the composition of the wool fat and of the quantity of acetone used
in the production possesses a melting point lying between 60-75° C. or above the
latter and consists preponderately of sebacic acids. If then to the filtered acetone
solution there is added the quantity necessary for the saturation of the still existing
sebacic acids, of a concentrated alkali or earth alkali solution, the greatest part
of the sebacic acids is separated as soaps, which can easily be filtered and washed
with acetone. Also the production of the high melting combinations can be left
and as hereinbefore described the sebacic acids can be separated as soaps.
The operation can be done at the usual temperature or with heat but in the
latter case it must be left to cool before filtration.
The filtered soaps can be used as such or be worked in the known manner as
sebacic acids.
Instead of separating the soaps from the acetone solution the sebacic acids can
be previously transformed into soaps by treating the mixture with alkalis or earth
alkalis and then be dissolved out with acetone.
In the same manner can be used instead of acetone: methyle-aethyle- or amyl-
alcohol, fusel oil, ether, chloroform, acetic ether and bisulphide of carbon.

page_text: 4. The solution separated in all cases from the soaps contains besides the fat
alcohols also sebacic acid soaps which can be separated for the most part by
evaporizing one part of the solvent and by congelation. The finally resulting
solution is freed by distillation from the solvent and the residuum which contains.
besides the fat alcohols also small quantities of sebacic acid soaps, is cleaned
further in the following manner.
It is boiled with diluted alcohol and is then kneaded with the same solvent and
finally with water, whereby the sebacic acid soaps are dissolved and in the beginning.
the wax like mass receives a softer consistence, combinations of the fat alcohols
being formed with water or the residuum after washing with diluted acids and the
water is submitted to distillation in or without a vacuum or with superheated steam
whereby the sebacic acids distil over first and then about 80% of the fat alcohols
as a thick oil, which for taking off any existing fat acids is kneaded at first with
dilute alcoholic ammonia or alkalis and finally with water, whereby there are
produced water containing combinations of salve like consistence. The thick oil
which goes over last at the distillation congeals to a hard wax like mass which can
serve as a substitute for bees wax and the residuum can be dissolved in benzine,
chloroform, ether, benzol, toluol or tar oils; the soaps can be taken off by washing-
with water the solvent can be distilled off and the resulting residuum the wool
fat alcohols can be separated by fractional distillation or crystallization in harder
or softer parts and the same can be transferred by kneading with water etc. into
the corresponding softer combinations. The mixture of the wool fat alcohols
or parts of their combinations with water can be used in pharmacy under the-
name of lanoglycerine.
Having now particularly described and ascertained the nature of this said inven-.
tion and in what manner the same is to be performed I declare that what I
claim is
The improved processes for the production of chemical combinations from raw
wool fat in the following manner.
1. The separation of raw wool fat by alcoholic ammonia or by distillation into
neutral wool fat and sebacic acids or into one part containing preponderately
sebacic acids and into another part consisting of a mixture of sebacic acids and
fat alcohols.
2. The further separation of the last named mixture into nearly pure sebacic
acids and into fat alcohols mixed with a few sebacic acids by profiting from the.
quality of the alkali or with alkali or metal-soaps to dissolve with difficulty in acetone.
methyl-aethyle or amylalcohol fusel oil ether, acetic ether, chloroform, or similar
solvents whereby on subsequent crystallization from the said solvents, combinations.
melting between 60-75° C. may be obtained.
3. Clarifying the impure fat alcohols by boiling and by kneading with diluted.
alcohol and finally with water, or by washing the soaps out of fat alcohol
solutions, or by distillation in order to work them finally into lanoglycerine, free-
from water or in combination with water, all substantially as described and set.
forth.
Dated this 6th day of August 1806
HERBERT HADDAN & Co.,
18 Buckingham Street, Strand, London, W.C., Agents for Applicant..