Note: Descriptions are shown in the official language in which they were submitted.
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DESCRIPTION
The water distillation is the oldest way of distillation at which the material
is immersed in
water and boils together with it. It provides very good conditions for hydro-
diffiision. At
atmospheric pressure the temperature does not exceed 100 degrees C which is
friendly to
thermo labile components. It is irreplaceable for raw materials with high
degree of
sinking /rose blossoms, orange blossoms, ilang-ilang, etc./, for wild raw
material for
example such as ¨ in France, Spain and Italy- lavender; Indonesia-kananga;
China-
cinnamon and for strongly ground plant parts since it ensures permanent mixing
and
contact with the water steam. It is technically and economical advantageous
for raw
materials with low degree of ethereal oil content. The water distillation
disadvantages of
the old methods are: the yield is less, the water-soluble and highly boiling
components
remain partially in the water remaining in the apparatus, the hydrolysis of
the esters is
accelerated and the quality of the oil is lowered, in cases of ineffective
mixing the raw
material or the extracted from it water-soluble substances could burn over the
heating
surface of the apparatus and to render a side odour of the ethereal oil, the
duration of the
distillation id restricted by the water present in the apparatus and in cases
of a long
process it is necessary an additional filling up, the apparatus capacity is
not completely
used, a considerable amount of water is heated which at the end of the process
is thrown
away which increases heat and time consumption.
On Figure I is shown Water generator of boiling water for water distillation
soaking the raw material periodically, a process repeated many times with
intense
discharge of saturated steam with ethereal-oil fumes 1-Cylnidrical reservoir;
2- Cone
chamber; 3- Cylindrical chamber; 4- Circular curved pipe/Fig. 2-elevation
B/through
which passes pre-heated water from pipe 6. In its circular profile it is
exposed to
peripheral heating from a gas burner 136/ Fig 14/ and enters reservoir 1; 5-
Valve letting
through the water coining from pipe 6 only in the direction of supply and not
letting it
through in the opposite direction; 6- Pipe supplying the already heated water
to sponge 52
of cover 42 by means of a distributing cock 47- providing the hermetical
quality of
reservoir 1; 7-Water generator for boiling water; 8- Boiler for processing the
raw
material; 9- Separating cone-shaped grid aiming at maintaining a short
distance from
cover 143 but at the same time providing enough air space for effective
diffusion of the
boiling water; 10-Cock for draining reservoir 1; 11- Cock for regulating water
level in
reservoir 1; 26- Legs which ensure fixed coupling between cone chamber 2 and
the
bottom of the generator; / the bottom shouldn't be thinner than 2 mm in order
to endure
continuous direct fire because although for a very short span of time it
remains dry
without water and under vacuum yet deformations are undesirable/, 143
Hermetically
welded /soldered/ upper lid of reservoir 1, concave on towards the reservoir
with an
opening in the middle with diameter equal to the diameter of cylindrical
chamber 3. To
143 is welded the upper part of 3 and the lower part of 3 to 2 and by means of
legs 26 is
the fixed coupling with the bottom.
Cone chamber 2 is in the form of a wide angular cone with low height in order
to
cover almost the whole bottom of the generator without touching it and at the
same time
to ensure a small quantity of water under it. In fact this solves the problem
with the
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heating of an enormous quantity of water. After 10-20 minutes of heating
starts the
boiling of the water with a rather characteristic noise. It is a result oldie
strong thermal
whirl of the water in chamber 2 vertically upwards, through chamber 3, through
grid 9
and the soaking of the raw material with boiling water. With the
intensification of the fire
under the influence of the weight of the water in reservoir 1 and the strong
thermal whirl
in chambers 2 and 3 in vertical direction upwards from chamber 1 enters new
water from
chamber 2. It is heated in chamber 2 and in chamber 3 a permanent flow of
boiling water
towards the raw material is acquired and that goes on until the water from
reservoir 1
completely drains and soaks the overall raw material with boiling water / the
quantity of
water in reservoir 1 is calculated as to be enough for soaking of the overall
working
capacity of the boiler having in mind the quantity of the material /raw
stuff/. After that
occurs a momentary sucking back of the water from the raw material moving back
through grid 9, chamber 3, chamber 2 in reservoir 1, and its duration is very
short
/momentary/. This is a result of the vacuum that has been created in reservoir
I, the lack
of water in chamber 2 and the weight of water pushed out by the thermal whirl
in the raw
material. This unique process is repeated cyclically, many times and in a
direct ratio to
the intensification of the fire in burner 136 /Fig. 14/. From that follows
that the duration
of the cycle decreases with the increase of the fire. This manifold repetition
of the cycle
continues and in that way the temperature of the raw material levels with that
of the
water. With the gradual rising of the temperature of the raw material
accumulating
discharge and pushing out of saturated steam with ethereal oils occur. As a
result of that
gradual temperature rising and periodical absence of water all components of
the ethereal
oil released in the concrete temperature point are extracted. In boiling at
slow fire the
cycle may continue for about 5-10 minutes. This suggests that the process
itself can very
precisely be controlled and in that way the above mentioned disadvantages can
avoided
/whereas the maximum duration of 5-10 minutes depends on the working capacity,
the
smaller the working capacity the shorter the maximum duration is/. The speed
of the
hydrolysis of the esters is slowed down and by means of that disruption of the
direct
contact of water with the raw material are reduced the losses of the water-
soluble and
highly boiling components of the oil dissolving in water. This raises the
quality and the
volume of the extracted oil from the raw material. The intense whirl mixes the
raw
material and by means of the so formed construction there is no direct contact
of the raw
stuff with the heating bottom; this prevents burning of the material and
formation of a
side odour of the ethereal oil. With automated supply of the already heated
water through
pipe 4 the process becotnes incessant and it is not necessary to dispose of
the water in
reservoir 1 at the end of each process. This eliminates thermal energy and
time
consumption. Naturally if different raw materials would be boiled for each of
them there
should be clear water which is supplied by pipe 6 already heated. Yet before
the supply
of clear water from crane is drained the previous water. The technological
process
constructed in that way with permanent movement of water through the heated
surface
does not allow any burning.
It is known that water has the highest degree of density at 3,98 degrees C and
while heating up to 100 degrees C at zero above sea-level height its
temperature
expansion changes its volume by narrow margins almost equal to zero. Water is
non-
contractible. After 100 degrees C it transforms into steam expanding its
volume
approximately 1670 times. The uniqueness of the method can compared to
pulsating
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heart-as the water the heart muscle and the discharged saturated steam with
ethereal oil is
the blood pushed out by the heart. The raw material exposed at intervals to
the influence
of the temperature pressure and the cyclically repeated vacuum is a kind of a
mechanic
maceration which helps for the easier bursting of the oil depository in the
processed
plants /raw materials/.This helps for the maximum extraction of ethereal oil
by means of
the new method of water distillation
Distillation method in which through a layer of material passes steam is
called
steam distillation which can be formed inside the very apparatus /water and
steam or
water-steam distillation/ or the steam is supplied by a special steam-
generator. The steam
distillation with a separate steam-generator is the most widespread method and
it has the
following technological and economical advantages: the speed can be precisely
regulated;
steam with different pressure is used i.e. with different temperature
depending on the
specification of the raw material; the water-soluble components are distilled
too because
they do not get into water environment; the continuity of the process is
unlimited; the
extraction of the water-soluble non-volatile components from the material is
avoided as
well as the overheating of the material and of the same components on the hot
surfaces;
the hydrolysis of the esters is reduced to minimum as well as the other
destructive
changes of the ethereal oils;
Up to now the constructed distilleries for steam distillation have the
following
disadvantages: they are not mobile/transportable/; they require steam boiler
and
respectively qualified personnel; they are not applicable in cases of
materials with high
degree of sinking or finely ground since the steam creates passages /channels-
tunnels/
and it can not affect the material completely; in cases of material with high
degree of
sinking it is necessary to be mixed with inert non-sinking materials which
makes the
production more complicated and expensive; it is not convenient for
distillation of
materials with small quantity of ethereal oil in them due to the enormous
consumption of
steam; the warm water from the condensers is not used to the best advantage;
intense
formation of condensate which periodically must be drained which leads to a
partial
break of the process or to additional heating of the bottom aiming at the
reduction of the
condensate.
Variant of the steam distillation is the so called water-steam distillation.
With it
the steam is fomed in the apparatus out of water which is located under the
material and
is separated from it by a perforated grid. The steam is saturated and is under
atmospheric
pressure. Due to the small quantity of water that can be filled one-time
before the start of
the boiling the distillation is short-termed and in case of a continued
process it is
necessary to stop the process in order to fill up water or to return the
distillation water
back into the apparatus which technically and economically is inexpedient and
results in
quantity and quality losses of the ethereal oil. The highly boiling components
of the oils
are distilled with difficulty and not incompletely due to the low temperature.
Part of the
non-volatile water-soluble substances of the raw material get along with the
condensate
in the water and cause the formation of carbon deposits on the heating suiface
of the
apparatus which results in the formation of a side odours of the oil and
disruption of the
heat exchange with the water. The speed of distillation is difficult to be
controlled.
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On Fig. 3 is shown a steam generator for steam distillation which is compactly
joined to the distillery and this makes it mobile /transportable/. It is
placed under the grid
separating it from the processed material. It produces superheated steam under
100
degrees C in vacuum regime or over 100 degrees C dry saturated steam and up to
or over
150 degrees C superheated steam in pressurized regime; 4-Circular curved pipe
/fig.2-
elevetion B/ through which passes a pre-heated water from pipe 6.1n its
circular profile it
is exposed to peripheral heating from gas burner l36/fig.14/ and it enters
reservoir 139;
5- Valve letting through the water that passes through pipe 6 only in the
direction of
water supply and not letting through in the opposite direction; 6- Pipe
supplying already
heated water to sponge 52 of lid 42; 7- Stearn generator; 8-Boiler for
processing the raw
material; 9-Separating grid which at its ends has a compact, not perforated
band which
purpose is to restrict the formation of steain flow along the walls of the
boiler without a
direct contact with the raw stuff /the so called tunnels/; 10- Cock for
draining reservoir
139; 122- Cock for draining tar 14. 13-Manometer combined with thermometer;14-
Tar;
15- Nozzle of the steam generator; I 6-Steam; 17- Visual and sound indicator
for
correcting the water level in the steam generator; 18- Steam diverting pipe
welded
hermetically to the bottom and in its upper part between the hermetical
weldings of the
middle part of nozzle 15 and the upper lid of the generator 140 there are
steam diverting
outlets along the circumference of the pipe; 19- Steam diverting pipe passing
though the
middle part of nozzle 15 and welded hermetically to it, suspended in pipe 18
and in its
lower part ending with a cone; 20- cone chamber; 21- Cylindrical chamber; 22-
Cone-
shaped platform; 23- Pipe diverting the steam towards a separating and steam-
diffining
grid 31; 24-Cock controlling the steam supply; 26- Legs ensuring fixed
coupling between
the cone chamber 20 and the bottom of the bottom of the generator; / the
bottom
shouldn't be thinner than 2 min in order to endure continuous direct fire/;
138 Pressure-
relief valve; I39-Reservoir of the steam generator; 140- Upper lid of the
steam generator.
With the steam generator are used the same methods of thermal whirl of the
water
heated in the cone chamber 20 whirling in an upward direction through the
cylindrical
chamber 21. It disperses on the cone platform 22 which stops the boiling
water. The so
designed construction helps for saving time and thermal energy, heating a
small quantity
of water and for an intense discharge of steam. The overflow of the boiling
water from
the cone platform 22 ensures great discharge of intensely saturated steam. As
the water
overflows it goes back, as a result of which a circular heat exchange occurs
with the basic
water in the reservoir 139. The released steam from the cone platform 22
passes through
the holes made on the lid 140 around pipe 18, and the holes made along the
circumference of pipe 18 in the lower part of nozzle 15. lt enters pipe 18 and
directs
downwards to the heated bottom in the lower part of pie 18. There the steam
superheats
and is drawn by the cone in the lower part of pipe 19, which ensures a larger
heating
surface for the steam. Through pipe 19 vertically upward it enters in a
diffuser with
circularly located outlets along the circumference of the nozzle 15. ln that
way the
equally distributed superheated steam is supercharged and through grid 9 it
enters in the
processed raw material. The holes along the circumference of pipe 18 are
located in the
highest point of the lower part of nozzle 15. The water level in reservoir 139
is calculated
so that without additional filling up the water to be enough for the boiling
of 3 boilers of
raw material. At the same time the volume of the water should be smaller than
the
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volume of half of the chamber of reservoir 139. The aim is when emptying the
boiler
from the material, after boiling / it is in a biased position that is more
than 90 degrees/
and if the water is more than the have volume of reservoir 139 there is a risk
of entering
into the cylindrical pipe 18.. The water in the process of boiling will be
pushed out
through nozzle 15 in the tar and that will disrupt their quality. After the
experiments that
have been made with an empty boiler without any material and under the maximum
thermal traction of burner 136 /fig.14/ steam temperature has been reached of
145
degrees C with fully open cocks 56, 57 and 58 between lid 42 and balancing the
pressure sponge 52 /fig. 8 and 9/. This proves the good quality of the steam
generator
because depending on how compact the material is arranged, the maximum
temperature
increases in a direct ratio to the increase of the density. The cocks 56,57,
and 58 help
very precisely to control with what pressure and respectively temperature the
concrete
raw material to be processed. The temperature that the steam can reach exceed
150
degrees C with closed cocks 56,57, and 58 under pressure of 0,7 atmospheres.
With
seeds, in some cases with blossoms and finely ground materials, it is
necessary for the
stuff to be separated by grid-diffusers-31/ fig. 4,5 and 6/. This is necessary
with the
large working quantities. For example for 500 liters is needed one separating
grid, with
750 and 1000 liters two separating grids. The grids are used only when the
system is
constructed for steam distillation. In case of water distillation separating
grids are not
used. The grids are located towards the perpendicular of the boiler 8 /fig.4/
under 3
degree bias aiming at producing a better quality of stream-lining without
stopping the
released steam saturated with ethereal oils. The grids 31 /fig.5 and 6/ are
constructed with
a specific form to facilitate their assembly and disassembly .Technologically
they are
made by a compact impervious plane located below. It ensures the hermetical
quality of
separation between the discharged saturated vapour with ethereal oil from the
remaining
below processed material and the supplied steam for processing the material
above.
Between base 32 /fig.7/ a moistened paper gasket is placed over which is
placed a grid in
order to increase the hermetical quality of separation. The upper plane of the
grid is
perforated. The perforation as distanced from the periphery in order to
prevent the
formation of tunnels that may be fomied towards the walls of the boiler. The
two planes
are separated by rims located so as to ensure an even distribution of the
steam and not to
allow any bending of the grid under the weight of the material and its
pressing during
loading. The separating grids solve the problem with the mixing of the raw
material with
the inert materials. In that way the complications and raising the cost of the
process are
avoided. On fig. 4 is shown the working part of boiler 8, without the steam
generator/fig.3/ or the generator for boiling water /fig.1/. It is wrapped
with glass wool
33 which is pressed by wooden laths 34 tightened by braces 35. This thermo
isolation
has the purpose of ensuring better heat exchange between steam and material or
steam-
water and for economy of heat and time. The wooden laths also play the role of
reinforcement which strengthens the construction. They prevent the possibility
mechanical damage while loading or emptying the raw material. By steam
diverting pipe
23 steam is supplied to the next levels, which is regulated by cocks 24 and
25. Pipes 29
and 30 divert the steam saturated with ethereal oils to the highest part of
lid 42. Cocks 27
and 28 and 56,57 and 58 control the even processing of the material. With
different
combinations of opening and closing of cocks 24,25,27,28,56,57, and 58 it is
possible
very precisely to control the vacuum and pressure. Respectively the
temperature for
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CA 02760036 2014-07-23
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processing the material totally for the whole boiler or for a particular
separating level of
raw material. In case of any possible error or closing of cocks 24 and 27 a
safety valve
138 is activated which opens and prevents the system from excessive pressure.
The
angular profile is circular- curved metal shaped iron around which is plated
the upper
border of boiler 8 /of flat copper/.To the inner periphery of the upper part
of the boiler is
welded a circular-curved copper rim36, and along the outside periphery is
welded a
circular-curved copper rim 38. Thus between the rims 36 and 38 a furrow is
formed in
which there is a silicone gasket and lid 42 is placed. It tightens and
hermetically seals
with clamps 133/fig. 14 /. On fig.8 and 9 is shown lid 42 balancing the
pressure by
sponge 52. It has the form of a hemisphere and half of its surface has a water
jacket 53.
The water jacket is intended to have a maximum small volume with the purpose
of quick
heat exchange and cooling of the steam within very small temperature limits in
order to
prevent intense cooling and curdling of the steam. It is fed with water from
the cooler by
a hose 51 and is regulated by cock 50. The water jacket 53 can be replaced by
a spiral-
curved pipes the outlet towards cock 47 is the initial point with the
narrowest diameter of
the spiral and the entrance from cock 50 is the end of the spiral with the
widest diameter
in it. The distribution cock47 changes the direction of the outgoing water
from the water
jacket. In direction by hose 6 towards /the generator for boiling water (fig.
l) if the
distillery is designed for water distillation or steam generator (fig.3) if it
is a system for
steam distillation/ or by hose 48 towards radiator 129 /fig. I 4/ for cooling
and gathering in
reservoir 128 /fig. 14. This water jacket 53 has two main tasks in order to
acquire a
continuous and gradual cooling of the steam, which results in a good
aggregation of the
distillate. The purpose is to increase the diameter of the oil drops released
in the water of
the Florentine /an oil-separating vessel/. The other task when it is necessary
to feed new
water in the steam generator /fig.3/ or in the generator for boiling water
/fig.1/, the water
to be already heated to the possible maximum of the concrete situation. The
angular
profile 43 is a circular-curved shaped iron around which is plated lid 42
/made of flat
copper/.Compensating the steam-diversion pipes 44. The regulation of steam-
diversion
through pipes 44 is controlled by cocks 56,57, and 58. The main steam-
diverting pipe is
45. The manometer 46 for measuring the pressure. Straight rim in the form of
semicircle
functions as a reinforcement of sponge 52 to which rim 59 is welded with an
opening for
suspending the sponge on arm61 (fig.10 and 11). Cone chamber 54 to which
hermetically is welded a Hollander fitting with a nut 55 for creating a fixed
coupling
with the cooler 77 (fig.I 2). Base 56.
The so build construction of lid 42 with sponge 52 comes to be a basic and
important junction for the good work of the system. The large volume of sponge
52 and
at the same time the small diameter of pipe 45 helps for the balancing of the
pressure
with which the steam is supplied. Thus under the cone of lid 42 the system is
under
pressure , and in sponge 52 under the impact of the vacuum formed in the
cooler 77, the
pressure in sponge 52 is almost invariably equal to zero. This doesn't load
cooler 77 by
cocks 56, 57 and 58 it is possible very precisely to control the pressure
hence the
temperature needed for processing of the concrete raw material. Based on the
so formed
construction of work of cooler 77 at full power of cooling in sponge 52 is
formed a
strong vacuum and at a minimum supply of steam by the precise opening of cocks
56, 57
and 58 the system starts to work under vacuum. During the time of tests, when
the system
works under vacuum with remove clamps 133 /fig.14/ it is practically
impossible the lid
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42 to open until the vacuum doesn't fall down. When the water in water jacket
53 is
approximately equal to 40 degrees C then under the influence of the vacuum
formed by
the cooler in the material are extracted the thermo-labile components from the
ethereal oil
materials with temperature around 60 degrees C. At the experiments made by
supplying
the necessary volume of steam at a slow fire, the necessary degree of cooling
arid the
precise opening and closing of cocks 56, 57, and 58 the system working under
vacuum
can process the raw material from 60 to 100 degrees C. And vice versa when the
system
works under pressure , the water in water jacket 53 under the thermal
influence of the
steam supplied by pipes 45 and 44 almost boils. If necessary it is possible to
be supplied
by hose 6 to the steam generator /fig. 3/ or to the generator for boiling
water /fig.1/. In
that way is saved a lot of heat and time.
On fig. 10 and elevation D /fig.11/ is shown the basic idea during a working
process of loading and emptying of the raw material. The attention is drawn on
the
mechanical construction.
60-double-row bearing, ensuring the rotation around bar 68 of arm 61; 61-arm
on
which is hung lid 42; 62-rod which ensures a rectilinear movement of bar 68
vertically
upward with the purpose of taking the lid 42 out of the furrow of boiler 8; 63
fixture; 64-
rod which is firmly welded to a metal frame 72 which by nieans of a bearing is
located in
pipe 75; 65- arms reinforcing the triangular construction; 66-boltscrewed up
in a nut 73
and fixing the boiler 8 in a vertical position; 67-muff, ensuring hermetical
quality of the
grease and of the normal lubrication and movement of bar 68 in pipe 74; 68-
bar; 69-
sstep; 70- triangle construction, base; 71- vertical reinforced rim; 72- metal
frame,
ensuring monolithic connection between the boiler and the base; 73-nut in
which a bolt is
screwed, fixing the boiler in a vertical position; 74-pipe; 75- pipe with
friction bearing;
76-base welded on one side to pipe 75 and on the other to arms 65;
On fig. 12 is shown a cooler 77. This is a heat exchanging apparatus /
condenser/
which is intended to condense the vapour of the water and the ethereal oil and
to cool
them to a certain temperature. The most popular in industry have become
coolers of the
type pipe bundle and serpentine (worm-pipe). The cooler of the type pipe
bundle is
compact , with a large cooling surface , it is easy to be disassembled and
cleaned. It
allows higher speed of distillation due to the lower resistance of the steam.
As a result of
the quick trickling of the distillate and its falling down in the collector
the oil drops
become smaller, which is not favorable for the extraction of the oil in the
oil-separating
vessel /Florentine/. The cooling surface is not used completely because the
distillate
trickles down in streams. That's why it is recommended the theoretically
calculated
surface of cooling to be doubled. The advantages of biased coolers of the type
pipe
bundle in comparison with the vertical pipe-cased coolers is the stable
temperature
regime of work which once settled preserves for the rest of the process.
Practically it is
found out that I square meter cooling surface cools 20-25 liters distillate
for an hour.
The worm-pipe cooler is simple in construction and easy for repairing. The
condensation in it is facilitated by the constant change of direction of the
vapour. The
aggregation of the oil drops is better and improves the discharge of ethereal
oil in the oil-
separating vessel /Florentine/. The disadvantages are the practical
impossibility for
tinning of the inner pipe, larger volume than that of the pipe bundle, little
possibility to
increase the speed of distillation due to the shown resistance, only part of
the cooling
surface is used in the cooling zone that is why it is recommended to triple
the
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9
theoretically calculated surface for cooling. To improve the exploitation
parameters very
often it is resorted to a gradual narrowing of the section of the pipe in the
lower part
which results in a more efficient use of the cooling surface. At normal work 1
square
meter cooling surface cools for l hour 25-35 liters distillate with
consumption of cooling
water with an outgoing temperature of 70-80 degrees C. The worm-pipe coolers
so far
have been applied predominantly in the extraction installations and vacuum
apparatuses,
where it is worked with vapour that is cooled with difficulty.
5I-hose supplying the already heated water coming out of the cooler towards
sponge 52; 78-cock, regulating the supply of the outgoing water from the
cooler 77; 79-
cock, regulating the cold water towards the cooler; 80-hose, supplying the
already cooled
water from reservoir 128; 81-chambr with cooling water; 82 chambers 1, H, III,
IV, and
V through which passes the steam and a process of condensation takes place; 83
and 84-
pipes diverting the already condensed vapour /distillate/ containing ethereal
oil; 85-
Hollander part on the side oldie cooler 77, ensuring hermetical coupling with
sponge 52;
86- thennometer by means of which is controlled the distillation process; 87-
filter
gathering the deposition particles from the oil sacks, which is cleaned
periodically; 122- a
drip pipe diverting the distillate; 123- a tip pipe supplying distillate to
the oil-separating
vessel /Florentine/; 148 and 149 technological outlets with caps for cleaning
pipes 84 and
83.
The so designed construction of cooler 77 is consistent with above mentioned
advantages and disadvantages. With the two types of coolers- pipe bundle and
serpentine/
wonn-pipe/ the advantages are preserved and the disadvantages eliminated of
each of the
types. Chamber I is the primary calmer of the incoming vapour. The acquired
condensate
drains down through pipe 84 in chamber V and directs towards the outgoing pipe
122.
The vapour passes through chamber II, which has the forin of a frustum of a
cone where
it is further calmed down and the process of condensation goes on. In chamber
III the
vapour changes its direction vertically upward and at the same time meets the
abrupt
narrowing in the passage towards chamber IV. Pipe 83 diverts the condensed
vapour
/distillate/ into chamber V and so on. Pipes 83 and 84 function as a feedback
ensuring no
remaining distillate in the cooler. Pipe 84 diverts the distillate already
formed in sponge
52 and that is the reason for the construction of the Hollander coupling in
sponge 52. It
has a cone-shaped outlet aiming at no retaining of distillate in sponge 52.
Chambers IV
and V are formed on the outer side with a cylinder in which is inserted a
frustum of a
cone with its narrow ending upward to the chamber E. Thus in the upper part
between
them is formed a larger volume whereas downwards a narrowing occurs with the
aim of
congesting and increasing of the cooling surface. Practically chambers IV and
V come to
be a type of a generalized pipe bundle in which over the diameter of the
cylinder the
steam moving back upwards constantly changes its direction from chamber IV to
chamber V resulting in an intense process of condensation. At the experiments
made,
with one and the same measurements of the cooler with pipe bundle and this new
type
of cooler we acquired 5 liters distillate more for 1 hour at one and the same
working
regime of working of the system. We approached the results with the coolers of
the type
serpentine /worm-pipe/. The cooler is not vertical but biased and once set on
a definite
working regime it does not change. IT can work at high speed of distillation
and in that
relation it is facilitated mainly by chambers IV and V. There is a constant
change of
direction of the vapour which does not result in the decrease of the size of
the condensed
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CA 02760036 2014-07-23
oil drops. After the construction changes that have been made in comparison
with the
cooler of the type pipe bundle we made the way of the steam longer 3 times and
increased the heat exchange surface almost 50 %. This is so because in order
to increase
the surface with the pipe bundle it is the number of pipes that is increased
per one surface
= measure but this is done within certain limits because when the pipes
become too many
it is technically impossible to achieve a high quality welding of the pipes
which results
in many defects and the cooler becomes unreliable. Another thing that can be
made is to
make the pipes longer. This can be done within certain limits, too because the
overall size
of the cooler shouldn't be too big. Its mobility/transportability/ is affected
whereas the
aim is to increase its efficiency.
On 4.12-1 is shown a cooler 77 with the same measurements as those shown on
fig. 12 It is with much greater efficiency, can work with a higher speed of
distillation
without decreasing its quality parameters. With it a new method is applied-
that of the
impulse cooling at which by cock 152 and pipe 155 is supplied cold water to
the installed
in serpentine 156. ln the chamber formed by sections VI and VII, so that the
cold water
passing through the serpentine causes an intense process of' condensation. It
is the
finalizing part of the cooling so that gradualness of the general cooling is
acquired so that
there is no curdling /abrupt cooling/. This gradualness helps the aggregation
of the
distillate with large oil drops. Through opening 157 at the end of serpentine
156 the
heated water directs to the outgoing water from the cooler. The supply of the
cooling
water is regulated by cock 79 and when there are minimal changes in the
process of
cooling cock 152 is opened till the filling up of serpentine 156 with new cold
water. ln
that way periodically the supply is provide at a regular intervals of time. At
a high-speed
distillation or at distillation under vacuum , cock 152 can be permanently
open and
regulate the capacity of the supplied cold water. The designed construction
allows very
precisely and permanently to control the process of cooling. The steam from
chamber I
through pipe 159 enters the hemispheric distributing chamber 11. There it
changes its
direction to 180 degrees and then enters chambers III,IV, and V which are the
space
between the cylinder within a cylinder and which like terrace-like change
their size.
Consecutively passing from one to the another chamber the direction of the
steam is
changed. This helps the good quality of condensation of the steam and provides
the
necessary time for heat exchange. The cylindrical form of the chambers is a
kind of a
pipe bundle along which the condensed distillate drips from the upper part of
the chamber
and in its lowest part each of the chambers has a pipe diverting the
distillate to chamber
VII, the pipes 83, 153 and 154. Each of the pipes 83, 84, 153 and 154 has
technological
outlets for periodical cleaning with caps 148, 149, 150 and 151. The outside
wall of
chamber VIII is a cone which with the horizontal line joins a 3 degree bias.
The aim is to
ensure an unimpeded streaining of the condensed steam in it. In chamber VIII
the steam
once again changes its direction and enters the chamber from the sections VI
and VII
which are form with an outer wall cylinder and on the inner side there is a
built in
cylinder with a frustum of a cone. The chamber formed between the cylinder and
frustum
of the cone are the pointed on fig. 12-1 upper section Vi and lower section
Vii. The
outlets 157 serve for air freeing of the water chamber formed between the
terrace-like
chambers III, IV, V and chamber VI and together with outlets 158 they ensure
normal
heat exchange and diversion f the heated water towards the outgoing opening of
the
cooler. The construction designed in that way lengthens the steam path 5 times
and
= =
CA 02760036 2014-07-23
increases the surface of the heat exchange from 3 to 4 times / with the
increase of the
number of windings of serpentine 156./ The temperature of the outgoing water
from the
cooler reach 80-90 degrees C.
On fig. 13 is shown the oil-separating vessel-container /Florentine/ combined
for
light and heavy oils. Two-sectional glass module for primary check of presence
of
ethereal oil in the entering in Florentine distillate and a glass chamber for
edging the
already released ethereal oil.
The separating vessels /Florentine/ work on the principle of the
interconnected
vessels. They ensure a constant release of water and in some cases of oil. The
separation
of the components of the mixture in it becomes possible due to their practical
inability to
mix and the difference concerning their density. Depending on the relative
density of the
ethereal oil its layer is above the water or under it and respectively in a
separating vessel
for light oils, heavy oils or combined- both for light and heavy oils.
The separating ability of the receptacles for light oil is detemiined by the
ratio
K= VI, where
V2
K- the separating ability;
VI ¨ the velocity with which the oil comes to the surface, m/s;
V2- the velocity of sweeping along of the oil drops by the distillate
downward, m/s.
The speed of coming to the surface of the oil drops is determined by the of
Stoke's law:
V1=d2 (p2-p I )s4
181.1.
where d ¨is the equivalent diameter of the oil drops, m;
p1 -the density of the oil, kg/m3;
p2- the density of the water, kg/m3;
g- the acceleration of gravity, m/s2;
- the dynamic viscosity of the water, kg/ (ms).
At p2>p1 (light oil) VI is a positive, i.e. the oil conies to the water
surface.
At pl>p2 VI is negative, i.e. the oil sinks to the bottom of receptacle.
The velocity of movement of the distillate downwards depends on its capacity
and on the
working section of the receptacle, i.e. on the surface through which the
distillate drains
down.
Where Q- is the capacity of the incoming distillate, m3/s;
S- is the surface of the section of the working part of the vessel, m2.
It is accepted that for a nomial part of the receptacle V2 shouldn't be
greater than 0,001
m/s at an unidirectional movement of the distillate and the ethereal oil,
while at an
polydirectional 0,0005 m/s.
From the above pointed formulas it is seen that the better separation of the
oil is ensure at
a lower velocity of distillation , larger drops of the ethereal oil, greater
difference in the
_ .
CA 02760036 2014-07-23
12
density of the oil and water and small viscosity of the water. The last two
factors depend
on the temperature of the distillate. The more the temperature rises the more
the
difference between the density grows and the viscosity of the water decreases,
which
facilitates the separation of the oil from the water. Knowing that water at
3,98 degrees C,
two molecules water unite in one molecule (1-120)2 then the water has the
greatest
density. The size of the drops of the ethereal oil depends on the speed of
condensation.
The gradual condensation favours the formation of large drops of ethereal oil.
The high
temperature of the outgoing from the coolers cooling steam allows the gradual
condensation.
It is accepted that the capacity of the separating vessel of the periodical
functioning apparatuses at average speed of distillation is enough t be 2-3 %
of the
capacity of the distillation apparatus. For the good quality of separation it
is necessary the
distillate to stay in the vessel at least 15-20 minutes.
The separating vessels are usually located one per distillation apparatus but
in case of
expensive oils two vessels are located consecutively. The second has a
controlling
function. When working with expensive oils it is usually resorted to gathering
the
material from all the apparatuses in one bigger receptacle, which results in
less smearing,
losses due to evaporations and pollution.
Florentine fig. 13: 87-periodically cleaned filter gathering the depositions
and
particles from the oil sacks; 88-cover hermetically sealing glass chamber 89,
in which the
primary edging is made and is determined the thickness of the oil ring of the
entering
distillate in the oil-separating vessel. By closing of cock 90 periodically a
test is made for
the oil content in the distillate; Thus by means of testing samples is
controlled the
duration of the process of boiling; 91- module for periodical edging; 92, 114
and 115
silicone, ensuring the hermetical sealing of the connections of the glass
modules with the
respective modules of the Florentine; 93-pipe through the distillate is
supplied to the
working cone vessel 107, ending in its lower part with a perpendicular spoon
94, by
which the direction of movement of the distillate is changed vertically
upward. In that
way the trajectory of movement of the distillate is prolonged and the time for
oil
discharge; 95-a cock which under nornial working conditions is closed and when
necessary can be used for transferring the distillate into a second separating
vessel or for
direct use of the ethereal-oil water; 96- a cock which is constantly open and
is closed only
when cock 95 is open or when is made a high-speed draining of the already
separated
light oil. Then both cocks-95 and 96 are closed so that the entering
distillate in 107 raises
the level only in chamber 107, whereas the level of the liquid in chamber 121
does not
change. In the process of permanent incessant draining of the light oil by
half-closing of
cock 96 the capacity of the entering distillate is regulated through cock 96
in chamber
121 to smaller than the capacity of the distillate entering from pipe 93. In
chamber 107
this leads to a gradual raising of the level only in chamber 107 and a
continued draining
occurs by edging in glass chamber 113 of constantly releasing ethereal oil; 97-
hollander
technological coupling which provides easy assembly and disassembly if cock 96
becomes defective; 98- a cock for draining the already separated secondary
light oils; 99-
a cock with pipe 108 for diverting the water separated from the distillate /
at work it is
always open/; 100- cock for emptying or draining of the separated secondary
heavy
oils;101- a cock for draining of 107 or for heavy oils; 102- air-vent with
stopper 103 for
_ .
CA 02760036 2014-07-23
13
hermetical sealing. The stopper is removed during a process of non-high-speed
draining
of the released ethereal oil as cock 99 is closed resulting in raising the
level in chamber
118, that gradually starts to fill up. If the stopper 103 is not removed it
may cause
babbling with bubbles in the already separated light oil so this may disrupt
its clarity and
quality; 104-oil-diverting pipe of the already edged oil in chamber 125; 105-
heavy oil;
106- light oil; 107- a primary working chamber for oil-separation. It is
conformable with
the formula of decreasing sweeping in downward direction and that is why
chamber 107
has the form of an asymmetric frustum of a cone. The lower base of the cone is
bent
toward cock 101 with the purpose of normal gathering and draining of the heavy
oils
when such are processed; 108- a pipe intended to ensure the constant process
of overflow
of water sucking from the middle part of the Florentine 121 in order to be at
an equal
distance from the secondary light and heavy oils and not to affect the normal
heat
exchange sucking up the coldest water from below, 109- a cone pipe, an
overflow drain
of the water from the primary chamber 107 to the secondary chamber 121. The
construction of overflowing by means of the cone pipe 109 is made so as to get
a
difference between the levels of the liquids so that the level in chamber 107
to be higher
than the level in chamber 121 thus to preserve one of the basic ideas
referring the normal
heat exchange between the liquids in chambers 107 and 121. Not to disrupt the
interconnected vessels but at the same time to ensure a greater difference
between the
temperatures of the releasing light oil 106 and the temperature of the water
in the lower
part of chamber 121 must approach the temperature with which the water has the
greatest
density-3,98 degrees C. In that way is preserved the formula of the speed of
coming to
the surface of the oil drops, defined by Stoke's law V1=d2 (p2-pl)g, so that
the water to
18
be with the greatest density, but at the same time the temperature in the
upper part of
chamber 107 where the light oil is, to be the highest ensuring a process of
maximum oil-
release. If we accept that during a polydirectional movement of the distillate
and the
ethereal oil V2= 0.0005 m/s for 20 min in a vessel with cylindrical form , as
the section
is one and the same along the section of the column in the process of release
of the oil the
oil drops will pass a 60 centimeters column. That is why chamber 107 has the
form of a
cone , along the vertical plane the section is variable , towards the base the
section
enlarges from which it follows that V2 decreases. At V2-0.0004 for 20 min is
necessary
48 cm column with V2= 0.0003 for 20 min it is 36 cm column, etc. The narrowing
of the
section of the cone along the vertical plane causes the released oil drops to
accelerate in
their movement upwards, whereas the distillate moving downwards decreases its
velocity. The idea of the so designed construction is to achieve a maximum
high
parameter for VI and maximum low parameter for V2. Thus we achieve a maximum
ability of separation K and the Florentine is multifunctional , applicable to
raw materials
with small content of ethereal oil as well to materials with greater content
of ethereal oil.
Its quality parameters are not changed after the connection of more than one
distillery.
After the experiments that have been made with the Florentine with capacity
120 liters
three distilleries can be connected with working capacity of 1000 liters. 110-
thermometer; 111-hermetically sealing cover; 112- bolts with nuts screwed
tight and
ensuring the hermetical quality between the modules and the glass chamber 113;
113-
glass chamber which serves to exert visual control over separating oil from
water during
the draining of the oil in the dehydrator 124; 116- module with a small volume
of
=
CA 02760036 2014-07-23
14
chamber 125 with the purpose of making a direct edging of the oil. That is
also
convenient for processing of materials both with small content of ethereal oil
and with
greater content of ethereal oil; 117- a horizontal base for tightening between
modules
116 and chamber 107 oldie glass chamber I 13; I 19- vertical base; 120-
secondary light
oil;
On fig. 14 is shown the principle diagram of distillery:
126-water pump, the supply of cold water can be provided by interconnected
vessels
without a pump; 127-a pipe-sucker, 128- a tank for collecting the cooled
water; 129- a
radiator cooling the water with a vane 130; I 31- a hose supplying the cooled
water from
the radiator to the reservoir 128; 132- a silicone gasket between boiler 8 and
lid 42;
133- U-shaped clamps ensuring a hermetical fixed coupling between the boiler
and the
lid. Depending on the diameter of the boiler the number of the clamps 133
increases as
the diameter increases, too. They are located at 20-25 cm from each other. In
the process
of work the furrow formed between the periphery of the boiler and the lid is
poured
water. lf there are outgoing bubbles periodically the concrete clamps 133 are
tightened;
134- gas bottle /propane-butane/; I 35-a hose supplying the gas to burner 136.
I 37-sheet
iron cylinder perforated and keeping the heat to the bottom of the boiler and
at the same
time preventing the fire of burner 136 from draughts; 1 38-safety valve;
At the testing samples made for example with boiling SUMAC OIL-OLEUM
COTIN1 (OLEUM COGGYGRIAE)
Normally in Bulgaria it is derived from0.13-0.2I % ethereal oil, whereas we
achieved
0.24-0.26 %. Our research at Bulgarian rose-Kazanlak after the processing I
/one/ ton
dry material of sumac for the maximum extraction of ethereal oil from 21 % are
used up
400 liters distillate. With new method and the new technical solutions with
the distillery
was extracted 0.26 % ethereal oil and were used up 175 liters distillate which
is 2.29
times less of the produced distillate for extraction of a greater quantity of
oil compared to
the distilleries used up to now.
After the processing of SALVIA OIL in Bulgaria from OLEUM SALVIAE
SCLAREAE from the young plants reaching the height of 0.90-1.10 meters the
extraction
of ethereal oil that has been reached amounts to 0,22-0,25 cY0, and from the
second l .30-
1,70 meters up to 0,27-0,30 %. With OLEUM SALV1AE OFICINIAL1S in Bulgaria has
been reached extraction of ethereal oil up to 0,18-25 % as the upper limit
refers to plants
reaching the height of 1.50 meters. With the distillery has been extracted
ethereal oil
amounting to 0,30 % young material with height of 0.90 meters.
On fig. 15 and fig. 16 is presented a nylon profiled cloth with cylindrical
chambers 141 which are filled with water, then are sealed and rolled in order
to be frozen
in a freezer. It is used at work in the open field where the raw material is
in case of
necessity. For example as shown on fig. 16, the already frozen cloth is
wrapped around
the Florentine 121 and is tightened with belts 142. This saves time and
consumption of
cold water and the process of oil-separation is stable.
On fig. 17 is shown a triple unifying module for periodical edging. Analogous
to
module 91 to which three distilleries can be joined as the processes of each
of the
distilleries can be controlled and check by cocks 143, 146 and 147.
On fig. 18,19, and 20 is shown a device for boiling cohobation of secondary
water
or a billet transformed into pulp. Fig. 20 is barrel 144, which is placed in
the boiler over
the grid and a cylinder is inserted in it with a cone lid along the outer
periphery of the
CA 02760036 2014-07-23
upper part of cylinder 145. It is oriented as to be in the center of the
boiler and its lid to
enter in the furrow of the boiler pressed by lid 42 and tightened by clamps
133. The
diameter of barrel 144 is a little bit bigger than that of 145 so that the
space between the
barrel and the cylinder is small. It ensures an unimpeded passing through of
the
superheated steam through it reaching the bottom of the barrel 144 from there
sweeping
vertically upward and transforming the oil drops into vapour. The construction
is
designed so that the superheated steam wraps the overall surface of barrel
144. It heats
the liquid in it and the formed pressure makes the steam to pass through the
passage
between the barrel 144 and cylinder 145, it sweeps the oil drops before the
entire liquid
has started to boil with a very characteristic babbling. The quantity of the
liquid can be to
the maximum of 2/3 of the capacity of the barrel. This is so because the
pressure of the
steam pushes out the liquid which is in the space between the barrel and the
cylinder in
cylinder 145. The maximum pressure is up to 0.7 atmospheres , knowing that 0.1
atmosphere displaces 1 meter of the water column, This device makes the system
multifunctional and convenient for work and in that way the ethereal oil
production cycle
closes.
