the Yolk or Grease of Wool.
Year: 1884

page_text: the Yolk or Grease of Wool.
[Communicated from abroad by Charles Viollette, Professor of Chemistry, and
Dean of the Faculty of Sciences, of Lille, Alphonse Buisine, Professor of
Chemistry, of Lille, and Alexandre Vinchon, Manufacturer, of Roubaix, all
in the Republic of France.]
I, WILLIAM HENRY BECK of 115 Cannon Street in the City of London,
Consulting Engineer and Patent Agent, do hereby declare the nature of the said
invention for "A NEW OR IMPROVED PROCESS FOR OBTAINING USEFUL PRODUCTS
FROM THE YOLK OR GREASE OF WOOL to be as follows:-
و"
The yolk or grease of wool is a product of little value, which has not heretofore
been applied industrially to any great extent, and can generally be utilized only
as material for adulterating tallows, greases and other fatty bodies with which it
can be mixed. The chief reasons why this grease has not heretofore become a
commercial product are: its very special nature, which is not suited to the
ordinary uses to which the other fatty bodies are applicable, the impossibility of
utilizing it by applying the same modes of treatment as are employed for ordinary
fatty bodies, and the absence of a practical and remunerative process which would
allow of its being transformed into utilizable products.
The following process, forming the subject of the present invention, enables solid
white products, useful for stearine works, to be obtained from the yolk or grease of
wool, in proportions hitherto unknown, as also oleic acid completely saponifiable.
and suitable for the manufacture of soap.
The yolk of wool is not, chemically speaking, a grease. It is a mixture of neutral
principles that do not contain glycerine, which is the characteristic element of the
greases properly so called, which are all glycerides.
A further proof that this body has nothing in common with ordinary greases, is
that none of the reactions applied to greases in the manufacture of stearine and soap
give results with the yolk of wool; it is, in fact, a material of entirely special
composition, which must be classed outside greases properly so called.
The yolk of wool contains the different fatty ethers of the cholesterines, oleate,
stearate, etcetera of cholesterine and of iso-cholesterine and, besides these, according

page_text: to recent researches of the inventors, a large proportion of cerotate of ceryle and
other fatty and waxy ethers, of similar structure, that is to say formed by the
combination of a fatty acid with a solid alcohol, insoluble in water. It is
therefore evident that the reactions applicable to the ordinary greases cannot give
results with this product, which differs so much from them in composition.
•
According to this present invention the different principles which enter into the
composition of this body are divided into their elements by saponification by
means of powerful agents such as the caustic alkalies at a high temperature.
In practice the inventors prefer to use for the solution solid soda in cakes
because the employment of lyes complicates the process by the introduction of
water which must be driven off before the reactions are produced.
The apparatus employed is composed of a boiler heated either by means of
a metallic bath which surrounds it, or by means of a "thermo-regulator" hot air
furnace. By these means overheating is avoided and consequent spoiling of the
products which might result from the direct employment of a furnace. The boiler
is furnished with a stirrer for mixing the mass during the whole operation: It is
also furnished with man-holes for the introduction of the materials, and with a
wide opening formed at the lower part of one of the ends of the apparatus for
withdrawing the products of the reaction. Thermometers show the temperature of
the mass and of the metallic bath.
A current of dry or superheated steam is led into the boiler for the purpose of
preventing the entry of air into the said boiler.
'
The volatile products of the reaction are first conducted into a dome on the
boiler, thence into a worm condenser surrounded with water, and furnished at the
bottom with an air tube for the escape of gases into the air.
The yolk in a perfectly dry state, and melted in the vat by the action of a worm
is led into the boiler by a pipe, the caustic soda in cakes or blocks as delivered in
commerce, and previously pulverized, is then introduced at one of the man-holes,.
in the proportion of one part of soda to four parts of yolk. The stirrers are
immediately set in motion by suitable driving pullies or other gear and the
temperature of the mass is raised to from 250° to 300°.
This temperature is maintained for a few hours, the agitation being constantly
kept up, after which the material is discharged from the boiler by the outlet near
the bottom into a vat placed below.
In this reaction the free fatty acids contained in the yolk (the yolk of wool
of commerce contains besides the natural grease, the fatty acids derived from the
soap employed in the washing) are first fixed without injury (altération) in the
state of alkaline soap, then the alkali at a sufficient temperature acts upon
the neutral ethers and splits them into their two components, fatty acids, oleic,
stearic, cerotic, etcetera, which are fixed in the state of soda soap, and into
àlcohols, cholesterines, cerylic, alcohol and others. These alcohols, liberated by the
saponification, are afterwards transformed or not at pleasure, and by the same
agents, into corresponding acids, as for example cerylic alcohol into cerotic acid.
When the reaction is completed the product is passed into vats where it is
treated with boiling water (3 to 4 litres of water per kilogramme of material).
The soda soaps are separated by cooling, and the water by drawing off and
pressure in filter-presses. The liquids drained of are concentrated, then calcined
in furnaces, and the major part of the soda in the state of carbonate is thereby
recovered from them.
The soaps are afterwards decomposed by acid, directly or after transformation
into salts of lime if it is desired to recover the whole of the soda.
The raw products which float are separated and, after washing, are submitted to
distillation in superheated steam. This distillation is carried out fractionally.
The first portions contain the most fusible products, the major part of the oleic
acid, accompanied with solid fatty acids which are deposited in grains; the oleic
acid which is completely saponifiable, and suitable for the manufacture of soap, is

page_text: separated by pressure. The second products, which are much less charged with
oleic acid, are treated in the same way with the addition of, oleic acid if that is
necessary for facilitating the crystallization in grains.
The products which follow, and which are very rich in waxy fatty acids are
treated in the same way with the addition of oleic acid to facilitate the pressure;
or better, as regards the easier separation of the liquid products, with the addition
of the usual solvents.
This mode of treatment yields a large proportion of solid fatty acids useful in
the steafine manufacture, more than 50 per cent of the weight of the primary
material employed, and also some oleic acid of high quality suitable for the
manufacture of soap; all commercial products produced by using a material
which has heretofore had no direct application and consequently no commercial
value.
The fatty acids thus obtained are of a special nature and distinguished by their
waxy appearence.
They contain, besides the ordinary stearic acid of the stearine manufacture, a
notable proportion of much higher fatty acids, the same as are found in waxes, and
especially cerotic acid.
The inventors have succeeded in isolating these latter fatty acids from the
mixture, and thus obtain a special product which is new in the stearine manu-
facture, and distinguished from the ordinary stearic acids by a much higher
melting point, and its waxy character.
The process consists in treating the raw acid derived from the yolk with certain
solvents such as the carburets.
The inferior fatty acids are more soluble in the hot state in the solvents than the
waxy acids and by a methodical treatment, these latter can be isolated in a
tolerable state of purity.
The process above described is equally applicable to the liquid and solid products
resulting from the distillation of the yolk.
In this process for the treatment of the yolk of wool, potash, in the solid or cake
form, may be substituted for soda; and these alkalies may be replaced by sodaed
or potassed lime in powder. In the latter case the following is a suitable way of
operating.
.
The dried yolk is mixed intimately, by means of a stirrer, with three quarters of
its weight of sodaed lime for example (containing, in the dry state two thirds of
lime and one third of soda). The mass, which immediately sets, is introduced into
flat retorts heated by means of a hot air "thermo-regulator" furnace to a
temperature of 250° or 300° which is maintained for from 10 to 12 hours. When
the reaction is completed the operation is finished as before, after removal of as
much as possible of the excess of lime by washing.
·
Dated this 19th day of Datahnu 1001

page_text: "
I, WILLIAM HENRY BECK of 115 Cannon Street in the City of London,
Consulting Engineer and Patent Agent do hereby declare the nature of the said
invention for." A NEW OR IMPROVED PROCESS FOR OBTAINING USEFUL PRODUCTS
FROM THE YOLK OR GREASE OF WOOL and in what manner the same is to be
performed to be particularly described and ascertained in and by the following
statement, reference being had to the accompanying sheet of drawings and to the
letters and figures marked thereon that is to say -
The yolk or grease of wool is a product of little value, which has not heretofore
been applied industrially to any great extent and can generally be utilized only as
material for adulterating tallows, greases and other fatty bodies with which it can
be mixed. The chief reasons why this grease has not heretofore become a com-
mercial product are its very special nature, which is not suited to the ordinary
uses to which the other fatty bodies are applicable, the impossibility of utilizing it
by applying the same modes of treatment as are employed for ordinary fatty
bodies, and the absence of a practical and remunerative process which would allow
of its being transformed into utilizable products.
The following process, forming the subject of the present invention, enables solid
white products, useful for stearine works, to be obtained from the yolk or grease of
wool, in proportions hitherto unknown, as also oleic acid completely saponifiable,
and suitable for the manufacture of soap.
. The yolk of wool is not, chemically speaking, a grease. It is a mixture of
neutral principles that do not contain glycerine, which is the characteristic element
of the greases properly so called which are all glycerides.
.
A further proof that this body has nothing in common with ordinary greases, is
that none of the reactions applied to greases in the manufacture of stearine and
soap, give results with the yolk of wool; it is in fact a material of entirely special
composition, which must be classed outside greases properly so called.
The yolk of wool contains the different fatty ethers of the cholesterines, oleate,
stearate, etcetera of cholesterine and of isocholesterine and, besides these, according
to recent researches of the inventors, a large proportion of cerotate of ceryle and
other fatty and waxy ethers, of similar structure, that is to say formed by the
combination of a fatty acid with a solid alcohol, insoluble in water. It is therefore
evident that the reactions applicable to the ordinary greases cannot give results
with this product, which differs so much from them in composition.
According to this present invention the different principles which enter into the
composition of this body are divided into their elements by saponification by means
of powerful agents such as the caustic alkalies in a dry state at a high temperature..
In practice the inventors prefer to use for the solution solid soda in cakes
because the employment of lyes complicates the process by the introduction of
water which must be driven off before the reactions are produced.
The apparatus employed and shown in Figures 1 and 2 of the Drawing hereto
annexed is composed of a boiler a heated .either by means of a 'metallic bath b

page_text: "
which surrounds it or by means of a thermo-regulator "hot air furnace. By
these means overheating is avoided and consequent spoiling of the products which
might result from the direct employment of a furnace. The boiler is furnished
with a stirrer with arms c c for mixing the mass during the whole operation. It is
also furnished with man-holes d d for the introduction of the materials, and with a
wide opening f formed at the lower part of one of the ends of the apparatus for
withdrawing the products of the reaction. A thermometer g shows the temperature
of the mass and another thermometer h the temperature of the metallic bath.
A current of dry or superheated steam is led into the boiler by a pipe k for the
purpose of preventing the entry of air into the said boiler.
The volatile products of the reaction are first conducted into a dome a¹ on the
boiler, thence into a worm condenser. 8 surrounded with water, and furnished at
the bottom with an air tube s¹ for the escape of gases into the air.
The yolk in a perfectly dry state, and melted in the vat m by the action of a
worm m² is led into the boiler a by a pipe m¹, the caustic soda in cakes or blocks
as delivered in commerce, and previously pulverized, is then introduced at one of
the manholes & in the proportion of one part of soda to four parts of yolk. The
stirrers c are immediately set in motion by suitable driving pullies p p' or other
gear and the temperature of the mass is raised to from 250° to 300°.
This temperature is maintained for a few hours, the agitation being constantly
kept up, after which the material is discharged from the boiler by the pipe finto a
vat placed below.
In this reaction the free fatty acids contained in the yolk (the yolk of wool of
commercè contains besides the natural grease, the fatty acids derived from the soap
employed in the washing) are first fixed without injury in the state of alkaline
soap, then the alkali at a sufficient temperature acts upon the neutral ethers and
splits them into their two componants, fatty acids, oleic, stearic, cerotic etcetera,
which are fixed in the state of soda soap, and into alcohols, cholesterines, cerylic,
alcohols and others. These alcohols, liberated by the saponification, are afterwards
transformed or not at pleasure, and by the same agents into corresponding acids, as
for example cerylic alcohol into 'ccrotic acid.
When the reaction is completed, the product is passed into vats where it is
treated with boiling water (3 to 4 litres of water per kilogramme of material).
The soda soaps are separated by cooling, and the mother water by drawing off and
pressure in filter-presses. The liquids drained off are concentrated, then calcined
in furnaces, and the major part of the soda in the state of carbonate is thereby
recovered from them.
The soaps are afterwards decomposed by acid, directly or after transformation
into salts of lime if it is desired to recover the whole of the soda.
The raw products which float are separated and, after washing, are submitted to
distillation in superheated steam. This distillation is carried out fractionally. The
first portions contain the most fusible products, the major part of the oleic acid,
accompanied with solid fatty acids which are deposited in grains; the oleic acid
which is completely saponifiable, and suitable for the manufacture of soap, is
separated by pressure. The second products which are much less charged with
oleic acid, are treated in the same way with the addition of oleic acid if that is
necessary for facilitating the crystallization in grains.
The products which follow, and which are very rich in waxy fatty acids, are
treated in the same way with the addition of oleic acid to facilitate the pressure;
or better, as regards the easier separation of the liquid products, with the addition
of the usual solvents.
This mode of treatment yields a large proportion of solid fatty acids useful in the
stearine manufacture, (more than 50 per cent of the weight of the primary material
employed) and also some oleic acid of high quality suitable for the manufacture of
soap; all commercial products, commanding a regular and assured sale and produced
by using a material which has heretofore had no direct application and consequently
no commercial value.

page_text: The fatty acid thus' obtained is of a special nature and distinguished from the
.ordinary stearic acid of the stearine manufactories by its waxy character. It
derives this property from the presence of special fatty acids the same as are found
in waxes and especially cerotic acid.
This process also resolves satisfactorily the important question of the purification
of the wash waters from wool, a question which is interesting from many points of
view, and which has, until now, remained unsolved in consequence of the want of
a practical and remunerative mode of treatment.
The process above described is equally applicable to the liquid and solid products
resulting from the distillation of the yolk.
In this process for the treatment of the yolk of wool, potash, in the solid or cake
form, may be substituted for soda; and these alkalies may be replaced by sodaed
or potashed lime in powder. In the latter case the following is a suitable way of
operating.
The dried yolk is mixed intimately, by means of a stirrer, with three.quarters of
its weight of sodaed lime for example (containing in the dry state two thirds
of lime and one third of soda). The mass, which immediately sets, is introduced
into flat retorts heated by means of a hot air "thermo-regulator" furnace to a
temperature of 250° or 300° which is maintained for from 10 to 12 hours. When
the reaction is completed the operation is finished as before, after removal of as
much as possible of the excess of lime by washing.
Having now particularly described and ascertained the nature of the said
invention, and in what manner the same is to be performed, I declare that what
I claim is
First The treatment of the yolk or grease of wool with caustic alkalies in a dry
state at a high temperature as herein before described, such treatment comprising
a. The complete saponification of the yolk or grease.
b. The transformation of the alcoholic principles into their corresponding acids
and.
c. The production of novel fatty acids which are distinguished from the fatty
acids heretofore produced in stearine manufactories by having a much higher point
of fusion, and by their waxy character.
Second-The application of the treatment hereinbefore described to the liquid
and solid, products resulting from the distillation of the yolk or grease of wool.