Improvements in the Separation of Woolwax from Woolfat. and in the Preparation of Lanoline from the more Fluid Residue.
Year: 1892

page_text: The decision of the Chief Examiner, acting on behalf of the Comptroller, of the
8th day of January 1895, allowed, under Section 18 of the Patents, &c. Act,
1883, an Amendment of this Specification.
Date of Application, 4th Aug., 1892-Accepted, 10th Sept., 1892
COMPLETE SPECIFICATION (AMENDED).
Improvements in the Separation of Woolwax from Woolfat. and in
the Preparation of Lanoline from the more Fluid Residue.
I, REGINALD HADDAN of the firm of Herbert & Co. Patent Agents of
18 Buckingham Street Strand W.C. London do hereby declare the nature of this
invention a communication to me from abroad by Doctor Benuo Jaffé and
Dr. Ludwig Darmstädter of the firm of Benno Jaffé and Darmstädter of
Martinickenfelde near Charlottenburg Germany, Manufacturers and in what
manner the same is to be performed to be particularly described and ascertained
in and by the following statement :-
With
Woolfat consists principally of an intimate mixture or compound of ether com-
binations of cholesterines and isocholesterines with the various fatty acids.
certain of the fatty acids cholesterine and isocholesterine form hard wax-like ethers
of high melting point, while with others of the fatty acids they form compounds of
a softer and more easily liquifiable nature.
It has been previously found that woolfat contains wax-like constituents the
presence of which detracts from the employment of woolfat profitably for medicinal
use, and for this reason as well as to procure a wax-like material suitable for candle
making or other manufacture, attempts have been made to separate the waxy
constituents. It should however here be noticed that the waxlike product pre-
viously produced by the splitting up of the chemical combinations in the wool fat
consists simply of a mixture of cholesterine, isocholesterine and the higher fat
alcohols, and this material which is termed "cholesterine wax "is not the same as
the definite compounds, being the cholesterine ethers or isocholesterine ethers which
are separated by the present invention.
The process hereinafter described provides a method by which all the wax, that
is to say, the harder chemical compounds in the woolfat may be separated in an
unaltered state from the more fluid, and this in such a manner that first the hardest
and afterwards successively the less and less hard compounds are separated from
the residue so that by stopping the process at any desired point it is possible to
obtain a separated product of any hardness and a residual product of any degree of
softness within the limits of the qualities possessed by the extreme constituents, or
if desired in like manner to obtain from or divide the raw material into several
products differing in hardness.
The various combinations with the fatty acids do not separate each exactly
distinct from the others but substantially in groups so that the first separation gives
a mixture in which the hardest compounds predominate. The less hard compounds
then gradually separate while the softest compounds remain behind longest. It is
therefore possible to break off the separation at the point where on the one hand
the separated product will fulfil the requirements for its employment in various
industries especially as a substitute for beeswax, and on the other hand a soft fat

page_text: will remain suitable for further treatment for instance for the production of a
lanoline of better quality and properties than the wax containing product now
manufactured.
This process may be carried out very well with raw woolfat.
If woolfat, raw or otherwise, is dissolved in a heavier benzine, benzole, toluole,
xylole, ether, chloroform, bisulphide of carbon or turpentine oil, and to this solution,
methyl-or-ethyl alcohol is added, the woolwax above described which is insoluble
in alcohol separates out. By adding a smaller or larger proportional quantity of the
alcohol, a smaller or larger quantity of the compounds-cholesterine- or isochole-
sterine-ethers separate, the smaller the quantity separated the harder the product,
since as beforementioned the harder kinds are the first to separate. On the other
hand the more that are separated, the softer will be-the-residual product obtained
by evaporation of the solvent. By this process therefore there may be obtained
from-raw-wool fut products of any consistency from that of wax to that of soft fats
which are almost liquid at ordinary temperatures.
By further purification of the latter by the usual methods, a wool fut is produced
which possesses all the good qualities of that already to be had, especially the
property of taking up water, without the disadvantages which the presence of the
wax like constituents produces; this therefore gives an excellent lanoline.
In-place-of-using the above solvents and separating-media-another-class of
solvents may be employed for dissolving the raw woolfut, and principal among these
is fusel oil, which is known to consist principally of amylic alcohol with propylic
and butylic alcohols and isomers of these. There may also be used for solvents
the above constituents of fusel oil, nectone, nectio-ether and its homologues and the
lighter benzines. These bodies dissolve all the woolfat will be dissolved at the
temperature of its melting point. By cooling down these this solution for a few
degrees below the melting point a separation of the above described harder waxy
compounds, (the actual woolwax) begins, and proceeds exactly as before described
in the process where the alcohol is added, the cooling being in all respects
analogous to the addition of alcohol, a greater cooling producing a product of less
hardness. The manufacturer can therefore stop the cooling whenever the product
of desired consistency is obtained. The residue remaining in solution is treated
for the production of lanoline exactly as that resulting from the first described
method:
It may be remarked that the separation of the harder components from, the
solutions made in the solvents mentioned in the second-category-may be equally
well effected by the addition of alcohol, but inasmuch as the process of cooling is
cheaper and dispenses with the cost of afterwards recovering the alcohol-separately
from the solvent, the cooling process will donbtless be preferred when dealing with
this class of solvents.
The chemical process is exactly the-same-if-the-raw woolfat be subjected to the
solvent in either category, after the necessary amount of alcohol has been added,
the-softer-constituents only will then be dissolved and the harder will remain
undissolved, the process is also the same with the solvents in the second category
if the solution be made at a temperature which is equivalent to that to which the
hotter solution is cooled for separation.
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 ;-
4)-The-division of raw or cleaned woolfat into harder and softer components by
solution of the woolfat in the heavier benzines, benzole; toluole, xylole, -ether,
chloroform, bisulphide of carbon or turpentine oil and separation of the woolwax by
addition of methyl or ethyl alcohol, the softer matters being recovered by
evaporation of the-solvent.
2) The division of raw or cleaned woolfat into harder and softer components
by solution of the woolfat in fusel oil or its constituents, in-acetone, neetie-ether or

page_text: its homologues, or lighter benzines; separation of the harder wool wax by-addition
of alcohol or by cooling the solution below the temperature of the melting point of
woolfat; and recovery of the softer matters by evaporation of the solvent.
3) The division of raw or cleaned woolfat into harder and softer components-by
treatment of the same-with-one or more of solvents described mixed with alcohol,
or by treatment with a solvent in the second category at a temperature less than
the melting point of woolfat, and subsequently-recovering the matter from the
solution.
4) The method of producing lanoline by the division of woolfat into softer and
harder varieties of cholesterine or isceholesterine ethers and subsequent purification
of the softer of such-varieties.
+
HERBERT & Co.,
Agents to Applicant.