from Oleagenous Seeds.
Year: 1886

page_text: from Oleagenous Seeds.
I, ADOLF BRÜNSTEIN, of Moscow, Russia, Pharmaceutical Chemist, do hereby
declare the nature of this invention to be as follows:-
Heretofore alizarin oil has been exclusively prepared from oils extracted from
plants and animal fats which have been treated with sulphuric acid and then
neutralised with alkalis.
According to the present invention alizarin oil is obtained directly from
oleagenous seeds by the following method. The oleagenous seeds, preferably
ricinus seeds, (ricinus communis) are first freed from their outer cuticle by passing
them through a pair of smooth horizontal rollers or by any other suitable means.
The decortication inay however be dispensed with at the expense of some loss of
time and a larger consumption of sulphuric acid; after passing through the rollers,
the cuticles are removed from the seeds by any suitable screening operation. The
seeds are then passed through the roller mill consisting of three horizontal granite
rollers constructed in precisely the same manner as the roller mills employed for
grinding the mixture of cocoa and sugar in the manufacture of chocolate, the only
difference being that the front knife which removes the pasty mass from the last
roller is made of glass or wood and that there is provided behind the hopper,
through which the seeds pass between the first rollers, a glass bar, on which
rests a lead box which serves to distribute along the whole length of the rollers
the requisite quantity of sulphuric acid that flows into the box from a reservoir
above.
I have found that in using wood for these parts, such as fir scrapers, stirrers,
knives, &c. they will be effectually protected against carbonisation by the sulphuric
acid if oak or other dense wood, free from resin, and soaked in paraffin, be used.
The seeds are first passed twice through the roller mill without sulphuric acid
whereupon a thin stream of sulphuric acid (of at least 60 per cent. or, if available,
anhydrous) is caused to flow into the before mentioned lead box from which the
acid passes through channels on to the rollers. In this manner there is supplied to

page_text: the seeds treated, according to the percentage of oil therein, from 40 to 60 per
cent of sulphuric acid, the mass being caused to pass about 6 times through the
mill. This treatment with sulphuric acid must be effected slowly in order that
the mass does not become heated beyond 40 to 50° C. The completely sulphurised
mass is allowed to rest in a lead lined tank for some hours, when a thick layer of
the sulphurised oils will collect at the top, which is then decanted. At the bottom
a compact deposit is formed which contains from 6 to 8 per cent of oil of the seeds
treated. In order to obtain this oil there is poured upon the deposit cold water to
the extent of about 170 gallons to 10 lbs. of deposit which is stored carefully up
with the mass and this is then allowed to stand about two hours. The separate
acid water is then decanted and a fresh quantity of water is added to the deposit
to the extent of about three times the first quantity and, after suitable stirring, the
mass is again allowed to stand for about an hour; the second quantity of water
added dissolves the oil still contained in the deposit, such oil being readily soluble
as it contains but little acid. This last solution is mixed with the oils first
obtained and the mixture is allowed to stand from 12 to 24 hours. By the
addition of common salt the oil passes more readily to the surface. In some cases,
for instance, in the preparation of soda-oil, the addition of salt is indispensable.
After the mixture has been allowed to stand as described, the separated water is
allowed to flow off and the product is ready for neutralising by means of ammonia
or caustic soda according to requirements. Experiments have given the following
results.
1. Of the oils prepared in this manner there is about 10 per cent less in quantity
required than of the ordinary alizarin oil prepared from ricinus, while, at the same
time, it is quite equal to the latter as respects beauty and fulness of the color to
be obtained.
2. The preparation of the oils according to this method costs from two to four
shillings per pound of alizarin oil less than the cost of that prepared from ordinary
pressed oil.
3. The manufacture of the oil is simpler and the installation of the necessary
apparatus is available to every dyer on account of its cheapness inasmuch as it only
costs about th that of an ordinary oil mill.
4. In applying this method, two operations are simultaneously carried out,
namely the oil is extracted from the seeds and is converted into alizarin oil.
5. This method obviates all causes of illness in the operatives such as swelling
of hands which occur in the ordinary manufacture of ricinus oil by pressing,
whereby the operatives cannot continue work longer than two years.
On the accompanying drawings are shewn at Figs. 1 and 2 a side view and
plan of the three-roller mill of improved construction which is particularly suitable
for the practical carrying out of the described process. The peculiarity of this
machine consists in providing at the back wall of the supply hopper A for the seed
small angle irons a a Figs. 3 and 4 which support a glass bar b on which is placed
a box of rolled lead having, close against the side of the hopper, a row of holes
whereby the concentrated sulphuric acid entering the box through the pipe c
flows on to the first granite roller B of the mill. To ensure uniformity of supply
of the acid, there is provided on the bottom of the lead box a longitudinal pro-
jection over which the acid flowing into the box behind the projection overflows.
The hopper A is coated inside and outside with lead; at the end walls the lead
sheets are cut out in such manner, as shewn at Fig. 3, as to lie close against the
peripheries of the rollers B1 and B2. The lead plates are fixed in position by
means of iron plates d, coated with lead, and screws c, and can be adjusted by
lowering, according as their lower edges wear away, and be then again fixed.
In order to properly guide the plates they have each a vertical slot through which
the iron rails on the end walls of the hopper pass, which rails carry the screws c.
In order to obtain the mass in as homogeneous condition as possible, the following
arrangement is employed.

page_text: Above the hopper A is a reciprocating bar D, Figs. 1 and 2, which is provided
with stirring pegs g and which is moved to and fro in the guides of the frame E
by means of the connecting rod F and the lever G. The short end of this lever
engages in the helical groove of the cam H which is fixed on the axis of the
roller B and which thus imparts the reciprocating motion to the lever G which is
transmitted to the stirring bar D. The mass treated in this machine is removed
from the last roller B by means of a wooden knife I soaked in paraffin. The
metal checks between which this knife is fixed are protected against the action of
the acid by means of a lead plate i. The cheeks are arranged to swing upon the
trunnions and are provided at the ends with small projections through
which the adjusting screws m m pass, whereby the position of the knife I may be
altered at will. The middle roller B revolves in fixed bearings while the bearings
of the rollers B1 and B are adjustable, so that the outer rollers can be moved
nearer to or farther from the middle roller. For this purpose the bearings of the
outer rollers are connected by rods n n with the eccentrics oo on the axes p p.
On the ends of these axes are worm wheels qq gearing with worms rr, by
rotating which, by means of the handles s, the above mentioned adjustment of the
position of the rollers B¹ and B³ is effected. K is a box or channel into which the
mass falls.
Instead of effecting the simultaneous crushing of the seeds and sulphurisation of
the mass as is done in the above described machine this may also be used solely
for the crushing operation, and the sulphurisation of the mass be effected in a
special apparatus.
Figs. 5 to 11 shew two arrangements of apparatus for effecting the sulphu-
risation of the finely divided mass. The apparatus shewn in vertical section
and plan in Figs. 5 and 6 consists of the stationary wood vat L resting on
supports M and filled with water for cooling the mass during the sulphuri-
sation. In order to effect a more perfect cooling, this water may be caused to
flow through the vat periodically or continuously. In the vat is contained a
lead coated iron receptacle N, carried by columns N¹, and which serves to
receive the mass to be sulphurised. A vertical axis O passes centrally through
the vat L and receptacle N and receives rotary motion through the bevil wheels Q
and driving pulleys P. The upper end of the axis carries two sets of arms R R
from which stirring bars S S pass down into the receptacle N. A ring U of angle
iron coated with lead and carried by supports T T carries a circular trough, which
has, at bottom, a projection for the purpose of uniformly distributing the sulphuric
acid supplied through the pipe V. This acid flows slowly through holes formed in
the inner angle of the trough into the receptacle N where it mixes with the
crushed seeds contained therein. As soon as the sulphurisation is completed
scrapers X are fixed to the stirring bars as shewn at Fig. 7 and the discharge
opening Fig. 6 is open so as to allow the finished mass to flow off. In order to
ensure a uniform mixture of the mass, it is advisable to begin the stirring operation
with ordinary stirring bars as shewn at Fig. 5 and then to attach to the stirring
bars the straight knives Z-as shewn at Fig. 8. These knives cause the mass to be
lifted and to be forced through the openings formed between the stirring bars.
Fig. 9 shews partly a side view and partly a longitudinal section of a trough
shaped stirring apparatus in which the axis with the stirring bars is arranged
horizontally. Fig. 10 shews an end view and Fig. 11 shews a cross section of the
apparatus. This apparatus also consists of a wooden vat L¹ filled with water for
cooling the inner iron receptacle N¹ lined with lead and made of semicircular form.
A horizontal axis O' passes centrally through the receptacle N₁ and carries the
stirring bars §¹. Over the receptacle is fixed upon standards T an angle iron
beam V¹ coated with lead which carries a lead trough into which the concentrated
sulphuric acid flows and whence it issues drop by drop through holes into the
receptacle N¹. As, in this case, the stirring bars raise the mass to be mixed, there
are provided at the edge of the receptacle wooden sides J in order to prevent the

page_text: material from being thrown out, which sides are connected to the vat L' by means
of hinges J. This arrangement of the stirring apparatus has the disadvantage
that, for the purpose of removing the completed mass from the receptacle N¹ as
also for cleaning the latter the entire axis with the stirrers must be removed.
Fig. 12 shews a two-roller mill of usual construction which may be used for
freeing the ricinus seeds from their cuticles in the first instance, or simply for
crushing the latter, to be employed when the sulphurising process is effected
separately as described. The construction of this machine is not new although it
has not heretofore been employed for the decortication of ricinus seeds.
200
1000

page_text: from Oleagenous Seeds.
I, ADOLF BRÜNSTEIN, of Moscow, Russia, Pharmaceutical Chemist, 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:
Heretofore, alizarin oil has been exclusively prepared from oils extracted from
plants and animal fats which have been treated with sulphuric acid and then
neutralised with alkalis.
According to the present invention, alizarin oil is obtained directly from
oleagenous seeds by the following method. The oleagenous seeds, preferably
ricinus seeds, (ricinus communis) are first freed from their outer cuticle by
passing them through a pair of smooth horizontal rollers or by any other suitable
means. The decortication may however be dispensed with at the expense of some
loss of time and a larger consumption of sulphuric acid; after passing through the
rollers, the cuticles are removed from the seeds by any suitable screening operation.
The seeds are then passed through the roller mill consisting of three horizontal
granite rollers constructed in precisely the same manner as the roller mills
employed for grinding the mixture of cocoa and sugar in the manufacture of
chocolate, the only difference being that .the front knife which removes the pasty
mass from the last roller is made of glass or wood and that there is provided
behind the hopper, through which the seeds pass between the first rollers, a glass
bar, on which rests a lead box which serves to distribute along the whole length
of the rollers the requisite quantity of sulphuric acid that flows into the box from
a reservoir above.
I have found that in using wood for these parts, such as fir scrapers, stirrers,
knives &c, they will be effectually protected against carbonisation by the sulphuric
acid if oak or other dense wood free from resin, and soaked in paraffin, be used.
The seeds are first passed twice through the roller mill without sulphuric acid
whereupon a thin stream of sulphuric acid (of at least 60 per cent. or, if available,
anhydrous) is caused to flow into the before mentioned lead box from which the
acid passes through channels on to the rollers. In this manner there is supplied
to the seeds treated, according to the percentage of oil therein, from 40 to 60 per
cent of sulphuric acid, the mass being caused. to pass about 6 times through the
mill. This treatment with sulphuric acid must be effected slowly in order that the
mass does not become heated beyond 40° to 50° C. The completely sulphurised
mass is allowed to rest in a lead-lined tank for some hours, when a thick layer of
the sulphurised oils will collect at the top, which is then decanted. At the bottom
a compact deposit is formed which contains from 6 to 8 per cent of oil of the seeds
treated. In order to obtain this oil there is poured upon the deposit cold water to
the extent of about 170 gallons to 10 lbs of deposit which is stirred carefully up
with the mass and this is then allowed to stand about two hours. The separate
acid-water is then decanted and a fresh quantity of water is added to the deposit,
to the extent of about threo times the first quantity and, after suitable stirring,

page_text: the mass is again allowed to stand for about an hour, the second quantity of water
added dissolves the oil still contained in the deposit, such oil being readily soluble as
it contains but little acid. This last solution is mixed with the oils first obtained
and the mixture is allowed to stand from 12 to 24 hours. By the addition of
common salt the oil passes more readily to the surface. In some cases, for instance,
in the preparation of soda-oil, the addition of salt is indispensable. After the
inixture has been allowed to stand as described, the separated water is allowed to
flow off and the product is ready for neutralising by means of ammonia or caustic
soda according to requirements. Experiments have given the following results.
1. Of the oils prepared in this manner there is about 10 per cent less in quantity
required than of the ordinary alizarin oil prepared from ricinus, while, at the same
time, it is quite equal to the latter as respects beauty and fulness of the color to be
obtained.
2. The preparation of the oils according to this method costs from two to four
shillings per pound of alizarin oil less than the cost of that prepared from ordinary
pressed oil.
3. The manufacture of the oil is simpler and the installation of the necessary
apparatus is available to every dyer on account of its cheapness, inasmuch as it
only costs about th that of an ordinary oil mill.
4. In applying this method, two operations are simultaneously carried out,
namely the oil is extracted from the seeds and is converted into alizarin oil.
5. This method obviates all causes of illness in the operatives, such as swelling of
hands which occur in the ordinary manufacture of ricinus oil by pressing, whereby
the operatives cannot continue work longer than two years.
On the drawings accompanying my Provisional Specification are shewn at
Figs. 1 and 2 respectively a side view and plan of the three-roller inill of
improvised construction which is particularly suitable for the practical carrying
out of the described process. The peculiarity of this machine consists in providing,
at the back wall of the supply hopper A for the seed, small angle irons a a Figs. 3
and 4 which support a glass bar b on which is placed a box of rolled lead having,
close against the side of the hopper, a row of holes whereby the concentrated
sulphuric acid entering the box through the pipe c flows on to the first granite
roller B of the mill. To ensure uniformity of supply of the acid, there is provided
on the bottom of the lead box a longitudinal projection over which the acid flowing
into the box behind the projection overflows. The hopper A is coated inside and
outside with lead at the end walls the lead sheets are cut out in such manner, as
shewn at Fig. 3, as to lie close against the peripheries of the rollers B1 and B2.
The lead plates are fixed in position by means of iron plates d, coated with lead,
and screws e, and can be adjusted by lowering, according as their lower edges wear
away, and be then again fixed. In order to obtain the mass in as homogeneous
condition as possible, the following arrangement is employed.
"
Above the hopper A is a reciprocating bar D, Figs. 1 and 2, which is provided
with stirring pegs g and which is moved to and fro in the guides h h of the frame E
by means of the connecting rod F and the lever G. The short end of this lever
engages in the helical groove of the cam H which is fixed on the axis of the
roller B and which thus imparts the reciprocating motion to the lever G which is
transmitted to the stirring bar D. The mass treated in this machine is removed
from the last roller B³ by means of a wooden knife I soaked in paraffin. The
metal cheeks between which this knife is fixed are protected against the action of
the acid by means of a lead plate i. The cheeks are arranged to swing upon the
trunnions and are provided at the ends with small projections through
which the adjusting screws m m pass, whereby the position of the knife I may be
altered at will. The middle roller B2 revolves in fixed bearings while the bearings
of the rollers B¹ and B³ are adjustable, so that the outer rollers can be moved
nearer to or farther from the middle roller. For this purpose the bearings of the
outer rollers are connected by rods n n with the eccentrics oo on the axes ?? P.
On the ends of these axes are worm wheels q q gearing with worms 1 r, by rotating

page_text: which, by means of the handles s, the above mentioned adjustment of the position
of the rollers B and B is effected. K is a box or channel into which the mass falls.
Instead of effecting the simultaneous crushing of the seeds and sulphurisation of
the mass as is done in the above described machine this may also be used solely for
the crushing operation, and the sulphurisation of the mass be effected in a special
apparatus.
Figs. 5 to 11 shew two arrangements of apparatus for effecting the sulphurisation
of the finely divided mass. The apparatus shewn in vertical section and plan in
Figs. 5 and 6 consists of the stationary wood vat L resting on supports M and filled
with water for cooling the mass during the sulphurisation. In order to effect a
more perfect cooling, this water may be caused to flow through the vat periodically
or continuously. In the vat is contained a lead coated iron receptacle N carried
by columns N¹, and which serves to receive the mass to be sulphurised. A vertical
axis O passes centrally through the vat L and receptacle N and receives rotary
motion through the bevil wheels Q and driving pulleys P. The upper end of tho.
axis carries two sets of arms R R from which stirring bars S S pass down into the
receptacle N. A ring U of angle iron coated with lead and carried by supports T T
carries a circular trough, which has, at bottom, a projection for the purpose of
uniformly distributing the sulphuric acid supplied through the pipe V. This acid
flows slowly through holes formed in the inner angle of the trough into the
receptacle N where it mixes with the crushed seeds contained therein. As soon as
the sulphurisation is completed scrapers X are fitted to the stirring bars as shewn
at Fig. 7 and the discharge opening Y Fig. 6 is open so as to allow the finished
mass to flow off. In order to ensure a uniform mixture of the mass, it is advisable
to begin the stirring operation with ordinary stirring bars as shewn at Fig. 5 and
then to attach to the stirring bars the straight knives Z as shewn at Fig. 8. These
knives cause the mass to be lifted and to be forced through the openings formed
between the stirring bars. Fig. 9 shews partly a side view and partly a longi-
tudinal section of a trough shaped stirring apparatus in which the axis with the
stirring bars is arranged horizontally. Fig. 10 shews an end view and Fig. 11
shews a cross section of the apparatus. This apparatus also consists of a wooden
vat L' filled with water for cooling the inner iron receptacle N¹ lined with lead
and made of semicircular form. A horizontal axis o' passes centrally through the
receptacle N¹ and carries the stirring bars 8. Over the receptacle is fixed upon
standards T' an angle iron beam V₁ coated with lead which carries a lead trough
into which the concentrated sulphuric acid flows and whence it issues drop by
drop through holes into the receptacle N'. As, in this case, the stirring bars raise
the mass to be mixed, there are provided at the edge of the receptacle wooden
sides J in order to prevent the material from being thrown out, which sides are
connected to the vat L' by means of hinges J'. This arrangement of the stirring
apparatus has the disadvantage that, for the purpose of removing the completed
mass from the receptacle N¹ as also for cleaning the latter the entire axis with the
stirrers must be removed. Fig. 12 shews a two-roller mill of usual construction
which may be used for freeing the ricinus seeds from their cuticles in the first
instance, or simply for crushing the latter, to be employed when the sulphurising
process is effected separately as described. The construction of this machine is not
new although it has not heretofore been employed for the decortication of ricinus
seeds.
Having now particularly described and ascertained the nature of my said
Invention and in what manner the same is to be performed, I declare that what
I claim is :
1. The method of obtaining alizarine oil directly from oleaginous seeds, wherein
these seeds are first passed through a roller mill into which concentrated sulphuric
acid is at the same time made to How, after which the solid and liquid substances
are separated from each other by subsidence and decantation substantially as herein
described.

page_text: 2. The method of obtaining alizarine oil directly from oleaginous seeds, wherein
the seeds are first ground down to a finely divided condition in a roller mill, or
other grinding apparatus, the ground mass being then mixed in an incorporating
apparatus with sulphuric acid and treated as set forth in the preceding claim.
3. The use of three-roller mills for obtaining alizarine oil directly from the seeds,
such mills being provided with appliances for obtaining a uniform supply of
sulphuric acid, for stirring the compound and causing it to flow uniformly on to
the rollers and for regulating the distance between the rollers and the position of
the knife or scraper for removing the mass from the last roller, substantially as
herein described with reference to Figs. 1 to 4 of the drawings.
4. The use of apparatus for treating the ground seed with sulphuric acid
consisting of the combination of a horizontal or vertical incorporating machine
with a lead vessel through which the sulphuric acid is made to flow slowly,
substantially as herein described with reference to Figs. 5 to 11 of the drawings.
Dated this 1 day of October 1000.
ABEL & IMRAY,
Agents for the Applicant,
28, Southampton Buildings, London, W.C.