Improvements in the Treatment of Wool Grease and of other like substances, and of Derivatives therefrom.
Year: 1897

page_text: Date of Application, 14th Dec., 1897
Complete Specification Left, 1st Oct., 1898-Accepted, 19th Nov., 1898
Improvements in the Treatment of Wool Grease and of other like
substances, and of Derivatives therefrom.
We, JOHN HOPKINSON, of Marion Street, Bradford, Manufacturing Chemist,
THOMAS COWLING, of 26, Brook Street, Bradford, Grease Merchant, and
FREDERICK ILLINGWORTHI, of Heather Bank, Heaton, Bradford, Wool Comber, all
in the County of York, do hereby declare the nature of this invention to be as
follows:
―:
This invention is applicable to the brown grease which is obtained from the
washing or the backwashing of wool by treating the soap suds with acid or the
grease obtained direct from wool by solvents or any other grease containing
unsaponifiable matter. Also the same greases which have been distilled by super-
heated steam or in vacuo or by both combined.
Firstly, we partially saponify the raw grease by adding to it strong caustic soda or
caustic potash in solution say of specific gravity 1250 or thereabouts and boil the
mixture until the alkali is absorbed. We then add sufficient sodium cloride or
other soda salt in solution as will precipitate the unsaponified fat, and we allow
the same to repose for a few hours. The unsaponified fat, which forms a super-
stratum is raw lanolin or a base for it. The substratum is a mixture of soap and
fat alcohols; to separate these, after the removal of the superstratum, we dissolve
the mass in ethyl or methyl alcohol or methylated spirit and dissolve out the fat
alcohols portionwise from the soap with any solvent practically insoluble in alcohol.
For this purpose we prefer coal tar benzole. The fat alcohols are separated from
the benzole by distillation and are used for lubrication.
The soap
is finished in the way well known to soap boilers and is then ready
for either household or manufacturing purposes.
Secondly, we take the raw grease and saponify it completely by adding to it a
slight excess of caustic soda or caustic potash (which is ascertained by an analysis
of each batch) and ethyl or methyl alcohol or methylated spirit and subject the
mixture to a pressure of two atmospheres until the saponification is complete.
After cooling down, a solvent, practically insoluble in alcohol is added preferably
coal tar benzole, which dissolves the fat alcohol from the soap. The
soap is then separated from the solvents by distillation and is ready
for finishing a term well known to soap boilers and the next
day is ready for the frames, where it solidifies and is used either for household or
manufacturing purposes. The fat alcohol is also separated from the solvent by
distillation.
Thirdly, we take the distilled grease and saponify by a slight excess of caustic
soda or caustic potash and ethyl or methyl alcohol or methylated spirit and allow
the mixture to repose. A large portion of animal hydrocarbon oil forms a super-
stratum, the remainder being held in suspension or solution in the soap and
alcohol. After the removal of the superstratum, coal tar benzole or any other

page_text: suitable solvent is added portionwise until all the animal hydrocarbon oil has been
purged from the soap. The soap is freed from the solvents by distillation and is
ready for finishing. The solution of animal hydrocarbon oil is also freed from the
solvent by distillation, and is a valuable machinery oil. Instead of finishing the
soup we may acidify it with an excess of mineral or organic acid and obtain a
mixture of stearic and oleic acid, which when freed from the excess of mineral or
organic acid may be crystallised in bulk and subjected to hydraulic pressure to
separate the solid from the liquid fat acid. The latter is known in commerce as
olein. The stearic acid is now ready for the manufacture of candles and the oleic
acid either for lubricating wool or for making soap.
Dated this 18th day of December 1897.
WM. P. THOMPSON & Co.,
Of 6, Lord Street, Liverpool, Patent Agents for the Applicants.
Improvements in the Treatment of Wool Grease and of other like
substances, and of Derivatives therefrom.
We, JOHN HOPKINSON, of Marion Street, Bradford, Manufacturing Chemist,
THOMAS COWLING, of 26, Brook Street, Bradford, Grease Merchant, and
FREDERICK ILLINGWORTH, of Heather Bank, Heaton, Bradford, Wool Comber, äll
in the County of York, 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 is applicable to the brown grease which is obtained from the
washing or the back washing of wool by treating the soap suds with acid or to the
grease obtained direct from wool by solvents or in fact to almost any other greases
containing unsaponifiable matter, also to grease obtained by distilling these and
other greases or like substances.
Now by our invention we obtain the lanolin or the grease from which it is
made in great purity. We obtain also an extremely viscose oil consisting entirely
of neutral fat which is a remarkably good lubricant for heavy machinery, and we
further obtain a very pure form of soap..
We partially saponify the raw grease by adding to 100 lbs. of grease 18 lbs. of
caustic soda solution specific gravity 1250 or equivalent quantity of caustic potash
of specific gravity about 1250 and boil the mixture until the alkali is absorbed.
The amount of alkali required for this purpose is preferably about 50% of that
actually necessary to fully saponify the saponifiable fats in the grease. As this
amount differs with different greases and with the wool fat from different climates
it is impossible to give exact quantities, but the quantity required to fully saponify
it can be easily found by experiments or analysis of a small portion of each batch.
The mixture is boiled until the alkali is absorbed. We add sufficient chloride of
sodium or other soda salt in solution as will precipitate the unsaponified fat.
The exact amount of chloride of sodium can only be found with each, given variety
of fat by experiment but approximately 14 lbs. salt in solution to 100 lbs. of fat
operated on. The mixture is allowed to repose for a few hours. The unsaponified
fat rises and forms a super-stratum of anhydrous lanolin. The sub-stratum' is a
mixture of soap and fat alcohols in solution. The super-stratum is removed and
to the sub-stratum is added ethyl or methyl alcohol or methylated spirit in the
proportion of about three and a half times the original bulk of grease operated
upon, the methylated spirits being preferably of specific gravity 950. The object
of adding ethyl or methyl alcohol is to obtain a complete separation

page_text: of the constituents of wool grease, but this can only be done in
conjunction with saponification and the addition of benzol or other
solvent, insoluble in dilute alcohol. It is utterly impossible to com-
pletely separate neutral fat and soap by the application of alkalies in
aqueous solution, either in a state of hydrate or carbonate, the fat from the
apparently separated soap having about the same composition as the mixed fat
which floats on the top. We now add a solvent of fat alcohols preferably coal tar
benzol which does not dissolve soap but only dissolves the fat alcohols when the
soap is dissolved in methylated spirits or ethyl alcohol of the strength and quantity
named namely specific gravity 950 and 3 times the weight of the original grease.
This coal tar benzol is added a little at a time and thoroughly stirred up, the fat
alcohols and benzol rise to the surface and are skimmed off and the solvent
separated by distillation. The fat alcohols thus obtained are an excellent
lubricant. The soap solution is finished in the usual wellknown way of soap
boilers and is then ready for either household or manufacturing purposes.
Where it is not requisite to obtain the lanolin and fatty alcohols in separate
form, the process can be simplified by completely saponifying at start, say by
adding about 30 lbs. of solution of caustic soda, specific gravity 1250 or an equiva-
lent amount of caustic potash to 100 of grease but the exact amount is ascertained
by an analysis of each batch. The ethyl or methyl alcohol or methylated spirits is added
and the mixture is submitted to a pressure of two atmospheres until saponification
is complete. After cooling down to about 180 degrees Fahrenheit, the coal tar
benzol is added as before. This dissolves the fat alcohols cholesterin and
isocholesterin leaving the soap however with the methylated spirits as a lower
stratum. After standing for a time the upper layer is drawn or skimmed off and
if necessary further benzol added to the lower layer and again skimmed off till all
the unsaponifiable matter is withdrawn from the soap. Each of the two liquors is
distilled to separate the solvent as before. The upper layer produces a mixture
of fatty alcohols forming an admirable lubricant of extraordinary viscosity and the
lower layer a capital soap for household or manufacturing purposes. It is obvious
that if the entire process first described were carried out and the raw lanolin and
the fatty alcohols added together a mixture valuable for lubricating purposes
very similar to that above described in which the lanolin has been decomposed by
saponification and some of its constituents been removed would be formed.
In applying our process to the grease that comes over and is condensed when
animal or vegetable oils or greases are distilled we saponify it by a slight excess of
caustic alkali and add of ethyl or methyl alcohol or methylated spirits about three
and a half times the bulk of the grease operated on and allow the mixture to stand.
A large proportion of animal hydrocarbon oil rises and can be skimmed off.
After its removal coal tar benzol or other solvent of hydrocarbons is added a little
at a time and agitated with it and skimmed off until all the animal hydrocarbon
oil has been removed from the soap. The soap is now freed from the solvents by
distillation and is ready for finishing. In practice benzol to about one quarter
the bulk of the impure soap operated on is used. The solution of animal hydro-
carbon oil is also freed from the solvent by distillation and is a valuable machinery
oil. Instead however of finishing the soap in any of these cases we may acidify
it with an excess of mineral or organic acid in the manner well known and thus
obtain a mixture of stearic or oleic acid which may be crystallised in bulk and
submitted to hydraulic pressure to separate the solid (stearic) acid from the
liquid (oleic) acid. The latter is known in commerce as olein. The solid stearic
acid is now ready for the manufacture of candles, and the olein can be used for
lubricating wool or for making soap.
Having now particularly described and ascertained the nature of our said
invention and in what manner the same is to be performed, we declare that what
we claim is:
1. The process of treating wool grease and other like substances which consists

page_text: in partially saponifying with heat, separating the unsaponified fat, dissolving
the remainder in ethyl or methyl alcohol separating the fat alcohols by means of
a solvent such as benzol and distilling off the respective solvents.
2. The process of treating wool grease and other like substances which consists
in completely saponifying with addition of methyl or ethyl alcohol and separating
the fat alcohols by a solvent such as benzol.
3. The process of treating distilled grease which consists in saponifying, adding
methyl or ethyl alcohol, skimming off the hydrocarbon oil assisted if required by a
solvent such as benzol distilling off the solvents and obtaining soap or fatty acids
substantially as described.
4. The manufacture of lubricant and soap from wool grease or distilled grease
substantially as herein described.
Dated this 20th day of Santambar 1909
W. P THOMPSON & Co.,
Patent Agents, of Liverpool, Manchester, Birmingham & London.