Improvements in Refining and Separating Wool-fat into Sundry Constituent Parts.
Year: 1895

page_text: Date of Application, 14th May, 1895-Accepted, 27th July, 1895
COMPLETE SPECIFICATION.
Improvements in Refining and Separating Wool-fat into Sundry
Constituent Parts.
I, EMILE MAERTENS, residing at Nairagansett Hotel, in the City and County
of Providence, and State of Rhode Island, U.S.A Manufacturer, do hereby
declare the nature of this invention and in what manner the same is to be
performed to be particularly described and ascertained by the following statement'
and accompanying samples:
My invention relates to improvements in refining and separating wool-fat into
sundry constituent parts.
I have discovered that wool-fat extracted from raw wool by solvents or by other
agents or means may be separated or divided into two or more new products, both
or all being the constituents of said wool-fat.
By the employment of my improvement in this art or process of treating wool-fat,
five resulting products are obtained from wool-fat as follows: z.-the first three
products to be described term primary products and are referred to throughout
this Specification as No. 4, No. 1 and No. 3, respectively; and the other two
products I term intermediate products, the same being referred to herein as No 5
and No 2, respectively.
The object of my invention is to more thoroughly separate or divide wool-fat
into products possessing different properties and characteristics, so that the various
constituent parts of said wool-fat, wheu obtained in a comparatively pure and
isolated state, are in the best form to be put to the various uses for which each 18
best adapted
The melting point, solidity, specific gravity, and transparency of the several
products vary according to the degree of completeness with which they have been
separated from each other.
This separation is considerably affected by the temperature and concentration of
the solutions from which or by which they are extracted.
If the wool-fat, in whatever manner obtained, 18 not pure, one or more of the
resulting products will be affected thereby to the extent and in proportion to the
quantity and character of the impurities existing in said wool-fat.
When the wool-fat is obtained from the dried wool by hydrocarbou solvents and
is free from sweaty matter, metal coloring, water and other common impurities, the
piimary products obtamed by the processes described herein have been found to
possess the following physical properties:-
No. 4 product 18 an opaque solid, or nearly solid, and generally inodorous waxy
fatty matter of a whitish or yellowish white color, not soluble or but slightly
soluble in cold acetone or cold alcohol, but completely soluble in about 30 times its
volume of boiling acetone, at 60 degrees F., specific gravity about 96; melting
point usually about 122 degrees. The specific gravity and the melting point of
the re-precipitated product from its solution in boiling acetone will vary with the
class and condition of the wool to which the product owes its origin, and both the
specific gravity and the melting point are higher and the product harder the more
dilute and the higher the temperature at which precipitation is made to take place,
and this may vary between 32 degires F. or less and just below the boiling point
of acetone. That portion which precipitates at a lower temperature or greater
concentration is of a lower gravity and lower melung point. The extremes of
gravity so far observed range from 9.55 to 9.76, and melting points 91 degrees F.
to 138 degrees h.

page_text: No. product is a transparent or translucent fluid or semi-fluid at ordinary
temperatures, of a yellowish red to a dark wine or brown color (when impure or
discolored by metals, alkalis, hent, etc., it may be greenish or blackish and some-
what opaque), generally odorons and generally possessing a resinous and sticky or
gummy nature and is readily soluble in cold acetone and cold alcohol; specific
gravity at 60 degrees F.. usually a little greater than 10 (or water). In those
cases where resin 18 absent or nearly absent or where it has been removed the
fluidity is greater and the gravity less. When this product is dissolved in a dilute
solution of 76 degrees naphtha (e. 76 degrees Beauiné) the resinous matter which
it contains precipitates on standing.
No 3 product is an oily, transparent, translucent, semi-opaque or opaque fluid or
semi-fluid or semi-solid (according to temperature and somewhat according to the
class of wool to which it owes its origin), and is generally inodorous, freely soluble
in cold acetone, but is not soluble or but sparingly soluble in cold alcohol; its color
when pure but not bleached is reddish yellow to yellowish red or reddish brown
(when not pure or discolored by metals, alkalis, heat, etc, it may be greenish or
blackish), specific gravity at 60 degrees F. about 96 to 9-67, in cases observed;
melting point between 50 degrees and 80 degrees F. (one very dark impure sample
melting at about 86 degrees F.).
Chemically considered, wool-fat is a mixture or combination of "cholesterin "
or its isomers or allied substances or alcohols with various fatty acids or resinous
matters and sometimes of such matters in a free state; tho exact chemical relation-
ship of these as they exist in the original wool-fat on the sheep is doubtless very
complex and probably has never been accurately determined and in the nature of
the case may be undeterminable. In the wool-fat itsolt they no doubt vary under
different circunstances and may be considerably affected by the process or materials
used in its extraction or recovery, and of course therefore the chemical constituents
of the divided products will be proportionately affected thereby
After considerable investigation I am of the opinion that "true cholesterin" seldom
if ever exists in the free state in wool-fat when extracted from wool (in its natural
state) with chemically inactive solvents, and of comse therefore under such
circumstances it would not appear in any of the products herein described and I
do not wish to base any claim upon its presence in or absence from any of these
products, as even when present its solubility in cold alcohol probably depends upon
other questions than mere temperature.
In describing therefore the chemical constituents of the above described products,
it is sufficient to say that:
The first named product No. 4, consists principally of a mixture or combination
of certain ethers or fats of "cholesterin," its 18omers or allied products and other
alcohols, which combination or mixture is not soluble or but slightly soluble in
cold or hot alcohol and also which is not soluble o1 but slightly soluble in cold
acetone, but is fully soluble in about 30 times its volume of boiling acetone, and
from which that portion of the wool-fat which will remain freely in solution in
acetone at a temperature at least as low as 32 degrees F. has been practically
eliminated.
No. 1 product is principally composed of free fatty acids, certain fatty ethers and
of the resinous gummy and odorous constituents of the wool-fat so far as such
combinations or mixtures of substances have remamed or will remain freely 10
solution in alcohol at a temperature at least as low as 32 degrees F.
No. 3 product consists principally of a mixture or combination of certain ethers
of "iso-cholesterin," "cholestei in and allied substances (with little or no fatty
acids, resinous or odorous matters) which product is not soluble or but slightly
soluble in cold alcohol but which mixture or combination is freely soluble in cold
acetone at a temperature at least as low as 32 degrees F and by which reduction
of temperature that product herein described as No. 4 has been eliminated and also
from which that part of the wool-fat (herein called No. 1) which is fieely soluble
in cold alcohol has been eliminated.

page_text: The intermediate products No. 5 and No. 2, obtained by the processos herein
described, are combinations or mixtures of the foregoing so-called primary products.
The No. 5 product being a combination or mixture of products No. 1 and No. 3,
while No. 2 is a combination or mixture of products No. 4 and No. 3. The
physical and chemical properties of these two compounds will vary greatly with
the proportion of their component parts in the particular wool-fat manipulated.
No. 5 product 13 a transparent, translucent or semi-opaque fluid or semi-fluid
according to temperature; it is of a yellowish red to a dark wine or brown colo
(when impure or discolored by metals, alkalis, heat, etc, it may be greenish o
blackish) liko product No. 1, but to a less degree, it is generally odorous, and
generally possesses a resinous sticky or gummy nature
No. 2 product in an opaque, fatty matter of a yellowish or reddish yellow colou
(when impute or discolored by metals, alkalis, heat, etc., it darkens, even up to a
greenish or blackish color), and it may be solid, semi-solid or semi-fluid according
to temperature.
The specific determination of No. 5 is here based principally upon its solubility
in acetone at all temperatures, as low at least as 32 degrees F., and the separation
therefiom (No. 5) as hereinafter described of No. 1 product, by the latter's
solubility in cold alcohol.
The specific determination of No. 2 is here based principally upon its insolubility
or eparing solubility in cold alcohol and the separation therefrom (No 2) as herein-
after described of product No 3, through the latter's solubility in acetone
wherein it reminius dissolved at a temperature as low as 32 degrees F.
In carrying my invention into effect, that is the refining of wool-fat and the
production and separation from it of the said primary products, No. 4, No. 1 and
No. 3, I can employ what I term tho acetone-alcohol process That is to say, the
wool-fat is placed in a suitable receptacle and therem digested with cold acetone
(or if preferred hot acetone, the solution afterwards being cooled) until the latter
18 Saturated with the No. 5 product which it has extracted or dissolved out of the
wool-fat. This solution, in acetone, of No. 5 product is then decanted into 4
suitable vessel or still, the remaining wool-fat being again digested with acetone,
and this operation ie repented and continued until all the No. 5 product contained
In the wool-fat has been dissolved out and decanted into tho said vessel or still.
After the No. 5 product has thus been extracted and removed there will still
remain in the digester that part of wool-fat which is insoluble or but sparingly
soluble in cold acetone and cold alcohol, which latter part, when freed by
washing, distillation or evaporation of the acetone adhering to it, forms my said
product No. 4.
The No. 5 product, before referred to as having been dissolved out and decanted
with the cold acetone into the vessel or still, is a residuum obtained from the
distillation or evaporation of the said acetoue solutions decanted from the wool-fat
with which it has been digeated, as stated before.
My product No. 3, the same being one of the constituent parts of product No. 5,
is obtained by digesting the latter product (No. 5) in alcohol, then decanting the
resulting solution and repeating this operation until that part of No. 5 product,
termed by me No 1, and which is soluble in cold alcohol, has been removed from
the remaining part, and the latter when freed by distillation, evaporation or
otherwise from the said alcohol adhering to it constitutes the said product No. 3.
The product No. 1 1s obtained as a residuum of the distillation of evaporation of
the alcohol solution decanted from product No. 5 with which it has been digested,
as before described.
The said products, No. 1, No 3 and No. 4, can also be isolated or extracted from
wool-fat by the following process, which I sometimes employ and designate it as
the alcohol-acetone process. That is to say, wool-fat is first digested with cold
alcohol, the resulting solution ie then decanted, said operation being repeated until
practically all that part of wool-fat which is soluble in cold alcohol has been

page_text: removed from it.
This last named product is also soluble in cold acetone and 18
identical with No. 1 produrt made by the former or first-named process.
There now remains behind an undissolved product which 18 herein before
described as No 2, the same being composed essentially of a combination or
mixture of the previously described products, No. 4 and No. 3. Now, in order to
1solate product No. 3 from this mixture, the latter is digested with acetone; the
resulting solution is next decanted and this operation is repeated until the whole of
No. 3 product has been separated or extracted, thereby leaving behind as a
residuum the No. product. The thus extracted solution, carrying the said
No. 3 product, is further treated by distillation, or evaporation, to free it from the
acetone; the resulting product being No 3. The residuum, or No 4 product, is
in turn freed, by distillation, evaporation or otherwise, from the acetone adhering
to it; the thus resulting product being No. 4.
In order to more clearly indicate the characteristic solubilities of the several
products produced by my improved processes, the following graphical or tabular
arrangement is given.
In these Specifications, both ethylated and methylated spits are included in
the term "alcohol" but I prefer to use ethylated spirits, as I find the results
therefrom to be most uniform and best effected.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, I declare that what I
claim, 18:-
1st. The improved method or process of refining wool-fat and separating it into
certain constituent parts, the same consisting in treating it with acetone, thereby

page_text: separating from the wool-fat that part which is soluble in cold acetone anil
desiguated herein as product No 5, then decanting the resulting solution, thereby
leaving behind that part of the wool-fat which had not dissolved in cold nretone
and is designated herein as product No. 4, and then eliminating the acetone from
the said resulting solution to obtain the above named product No. 5, while the
undissolved part when freed from acetone forms the above named product No. 4,
substantially as berembefore described.
2nd. The improved method or process of refining wool-fat and separating it into
three constituent parts, which consists in mixing or incorporating acetone with
wool-fat and separating from said woul-fat that constituent part of it which 15
soluble in cold acetone and is herein desiguated as product No. 5, while the other
Constituent part helem designated as product No. 4 remains undissolved, then
eliminating the acetone from the soluble constituent part to obtain said
product No. 5, and from the residuary or undissolved part to obtain said
product No. 4, (the thus resulting two products being the only separated constituent
parts of the original wool-fat), then incorporating alcohol with said No. 5 product
to separate therefrom that part which is soluble in cold alcohol (which said soluble
part when freed from alcohol forms the product herein designated as No 1), and
leaving behind that part of said product which has not dissolved in cold alcohol
and winch when freed from its adhering alcohol forms the new product herein
designated as No. 3, the resulting products No. 1 and No. 3 being separated
constituent parts of said new product No. 5, substantially as hereinbefore
described
3rd. The method or process of refining wool-fat and separating it into three
constituent parts, which consists in mixing or incorporating alcohol with wool-fat,
then separating from said wool-fat by extraction that constituent part of it which
13 soluble in cold alcohol and is herem designated as No. 1 product, while the other
constituent part which is designated herein as product No 2, (and which is a
mixture or combination of the constituent parts of the products designated herein
as No 4 and No. 3) remains undissolved, then eliminating the alcohol from this
undissolved or residuary part (and designated as product No 2), and then incor-
porating acetone with it and separating therefrom by extraction that part which
is soluble in cold acetone and is designated herein as product No 3, and leaving
behind that part which remains undissolved and which when freed from acetone
forms the new product designated herein as No. 4, whereas that part which was
dissolved out with acetone when freed from the latter agent forms the new product
No. 3, substantially as her erubefore described.
4th. As a new article of manufacture the refined opaque solid or nearly solid,
and generally inodorous waxy and fatty product generally of a whitish or yellowish
white color herembefore described as No. 4 product, the same being insoluble or
but slightly soluble in cold acetone and cold alcohol but completely soluble in
about 30 times its volume of boiling acetone and which can be obtained as a
residuum from wool-fat after the latter has been freed by extinction with acetone
from its other constituent part (herein designated as product. No. 5) and which is
soluble in cold acetone, substantially as set forth
5th. As a new article of manufacture the refined opaque solid or nearly solid
and generally inodorous waxy and fatty product generally of a whitish or yellowish
white color herein before described as No. 4 product, the same being insoluble or
but slightly soluble in cold acetone and cold alcohol but completely soluble in
about 30 times its volume of boiling acetone and which can be obtained as a
residuum from the wool-fat product herein designated as No. 2, after the latter has
been freed by extinction with acetone from its other constituent pait which is
berein designated as picduct No. 3, which is soluble in cold acetone, substantially
as set forth.
6th. As a new article of manufacture the refined transparent, or trauslucent or
semi-opaque resinous, sticky and generally odorous fluid, semi-fluid or semi-solid
designated herein as product No. 5, the same being soluble in cold acetone and

page_text: being one constituent part of wool-fat separated by extraction from its other
opaque fatty, waxy, solid or semi-solid constituent pait which is designated herom
as product No. 4, which latter is not soluble or but slightly soluble in cold acetone,
substantially as set forth.
7th As a new article of manufacture the refined transparent, translucent or
semi-opaque, oily fluid, semi-fluul or semi-solid product froin wool-fat soluble in
cold acetone but insoluble or but slightly soluble in cold alcohol, and which can
be obtained by separation from the product designated herein as No. 5, when the
latter is digested with cold alcohol, and which new product remains undissolved by
such digestion and when freed from said alcohol constitutes the product designated
herein as No. 3, substantially as described
8th. Ae a new article of manufacture the refined transparent, translucent or
semi-opaque or opaque, oily fluid, semi-fluid or semi-solid product from wool-fat.
soluble in cold acetone but insoluble or but slightly soluble in cold alcohol, and
which can be obtained by digesting the product designated herein as No 2, (which
is a mixture of No 4 and No. products) with cold acetone, which leaves behind
undissolved the product herein designated as No. 4 and dissolves out the other
constituent part of said mixture, which when freed from acetone is the product
herein designated as No. 3, substantially as described.
9th. The improved method or process of rehning wool-fat and separating it into
two constituent parts, the same consisting in treating it with cold alcohol, thereby
separating from the wool-fat that part which is soluble in cold alcohol, and
designated herein as product No. 1, then decanting the resulting solution, thereby
leaving behind that part of the wool-fat which has not dissolved in cold alcohol
and designated herein as product No. 2, and then eliminating the alcohol from the
said resulting solution to form one product, while the undissolved part when freed
from alcohol forms another product, substantially as herembefore described.
10th. The improved process of refining wool-fat and separating it into two
constituent parts, which consists in mixing or incorporating cold alcohol, or hot
alcohol and subsequently cooling, with wool-fat, and separating from said wool-fat
that part which is held in solution in this cold liquor and designated herein as
product No. 1, while the other coustituent part of the wool-fat, and designated
hereu as product No. 2 remains undissolved or in suspension in said solution, then
eliminating the alcohol from the soluble constituent part and from the suspended
or residuary constituent part, the thus resulting two products being separated
constituent parts of the original wool-fat, substantially as described.
11th. As a new article of manufacture the refined opaque, fatty product,
designated heroin as product No. 2 and obtained from wool-fat after the latter is
freed from its other coustituents which are soluble in cold alcohol, substantially in
the manner as hereinbefore descubed.
12th. As a new article of manufacture the refined transparent or translucent
product desiguated herein as product No. 1 and composed of the constituents of
wool-fat soluble in cold alcohol and separated from the opaque fatty product,
forming the other constituent part of wool-fat, substantially in the manner as
herembefore described.