CA2759869A1 - Control the process of distillation under pressure or vacuum without use of vacuum pumps, distileries are with different volumes, they distilling a raw material in dry or liquid condition, extracting for second time essential oils from liquid results obtained after distilation - Google Patents

Abstract

This invention relates to control the distillation process for the production of essential oils using water or steam distillation in the processing of different materials in different sizes of the distillers under pressure and vacuum without use of vacuum pumps, in case of processing a sinking materials in distillers over 300 liters volume only in steam distillation the raw material is divided from grids diffusers, in case processing a raw material in liquid condition or processing on distillation leads from previous distillation is using cohobation attachment; precise control distillation process reduces the cost production of essential oils, produced distillate required for maximum extraction of essential oil percentage from the raw materials, is decreased by 2-2.5 times and the volume of extracted essential oil increased by 10-16%.

Description

DIVISIONAL APPLICATION (1) TO CA 0,242,1141 PETITION

CONTROL THE PROCESS OF DISTILLATION UNDER PRESSURE OR VACUUM WITHOUT
USE OF VACUUM PUMPS, DISTILERIES ARE WITH DIFFERENT VOLUMES, THEY
DISTILLING A RAW MATERIAL IN DRY OR LIQUID CONDITION, EXTRACTING FOR
SECOND TIME ESSENTIAL OILS FROM LIQUID RESULTS OBTAINED AFTER
DISTILATION

DIVISIONAL APPLICATION (1) TO CA 0,242,1141 DESCRIPTION

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.

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 (3XFig.3). In case of water distillation separating grids are not used (1)(Fig.l). The grids are located towards the perpendicular of the boiler (8)(Fig.4) under 3 bias aiming at producing a better quality of stream-lining without stopping the released steam saturated with ethereal oils. The grids (3 1)(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 formed 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 DIVISIONAL APPLICATION (1) TO CA 0,242,1141 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, 28, 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 pressure and vacuum. Respectively the temperature for 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.

Example:
Boiler (8) is divided in 3 levels, level 1 is treated with steam directly from the steam generator, level

2 is above level 1, level 3 is higher than level 2, If the cock (24) is closed is processed only level 1, if cocks (25 and 27) are closed is processed only level 2, if cocks (27 and 28) are closed is processed only level 3, if cock (28) is closed are processed Level I and Level 3, if cock (27) closed are processed level 2 and Level 3, if cock (25) is closed is processed level 1 and Level 2, if all cocks are opened and processed three levels.

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 rim (36), 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 i DIVISIONAL APPLICATION (1) TO CA 0,242,1141 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 cock (47) changes the direction of the outgoing water from the water jacket.
In direction by hose (6) towards (the generator for boiling water (fig.1) 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.14) 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 temperature 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 Tridicator (46) for measuring the pressure and temperature. Straight rim in the form of semicircle functions as a reinforcement of hemisphere (52) to which rim (59) is welded with an opening for suspending the sponge on arm (61) (Fig.10 and 11). Cone chamber (54) to which hermetically is welded a union connection fitting with a nut (55) for creating a fixed coupling with the cooler (77)(fig.12). Base (56). The so build construction of lid (42) with hemisphere (52) comes to be a basic and important junction for the good work of the system. The large volume of hemisphere (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 hemisphere (52) under the impact of the vacuum formed in the cooler (77), the pressure in hemisphere (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 hemisphere (52) is formed a strong vacuum and at a minimum supply of steam by the precise DIVISIONAL APPLICATION (1) TO CA 0,242,1141 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 (42) to open until the vacuum doesn't fall down. When the water in water jacket (53) is approximately equal to 40 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 C. At the experiments made by supplying the necessary volume of steam at a slow fire of burner (136)(Fig.14), the necessary degree of cooling and 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 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.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 (8) over the grid (9) and a cylinder is inserted in it with a cone lid along the outer periphery of the upper part of cylinder (145). It is oriented as to be in the centre 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 atm (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. It is constructed to the very distillery which makes it compact from the point of view of closing the production cycle at the production of ethereal oil products. The construction is designed in such a way that the superheated DIVISIONAL APPLICATION (1) TO CA 0,242,1141 steam wraps the overall surface of barrel (144), heats the liquid in it , while the formed pressure causes the steam to pass through the passage between barrel (144) and cylinder (145). As it reaches the bottom of the barrel (144) it changes its direction vertically upwards sweeping the oil drops before the possible boiling of the entire liquid. Thus there is a constant babbling without boiling of the liquid. The separation of the partially dissolved low-boiling components of the ethereal oil occurs or these are the swept oil drops that have entered the secondary water.
These belong to the first phase zone. By raising the temperature and due to that of the pressure occurs the second phase zone where the components are mutually non-soluble. Raising the temperature causes the boiling of the entire liquid and then sets the third phase zone and the extraction of the highly- boiling components of the ethereal oil.

At the testing samples made for example with boiling SUMAC OIL-OLEUM COTINI
(OLEUM
COGGYGRIAE) Normally in Bulgaria it is derived from 0.13-0.21 % 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 litres distillate. With new method and the new technical solutions with the distillery was extracted 0.26 %
ethereal oil and were used up 175 litres 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 % , and from the second 1.30-1,70 meters up to 0,27-0,30 %.
With OLEUM SALVIAE OFICINIALIS 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.

Claims (6)

1. For water or steam distillation a lid (42) with hemisphere (52) (Fig.8 and 9) is a unit for control the processing of raw material in the boiler (8) (Fig.4), the pipe (45) restrict passage of steam saturated with essential oils from (8) to (52), but in the hemisphere (52) with control of opening or closing on cocks (56.57 and 58) helps to balance the steam pressure in the boiler (8), when a cocks (56.57 and 58) are closed into (8) below the cone lid (42) a raw material is processed under positive pressure, but steam passed into (52) under the influence of the vacuum formed by cooling from water jacket (53) and cooler (77) (Fig.12-1) *pressure in the hemisphere (52) is equal to zero, by using the steam-diversion pipes (44) with cocks (56.57 and 58) very accurately is made control the temperature-pressure in the boiler (8), in processing high degree of sinking raw materials are use the pipe (23,29 and 30) for steam distillation to control of temperature-pressure for each level separated by grid-diffusers (31) (Fig. 4, 5 and 6) or in the control processing of material in liquid condition using cohobation device (144 and 145) (Fig. 18); when (77) and (53) are working at *full power of cooling into the hemisphere (52) is formed a vacuum, by opening the cocks (56, 57 and 58) the vacuum in (52) suck out the steam from the boiler (8) and the pressure is negative under the lid (42) into boiler (8), from that moment the raw material begin processing under vacuum without the use of vacuum pumps, when maintaining * speed of cooling vacuum into (8) is constant.

2. The device of claim 1, to avoid with high degree of sinking raw materials or use finely ground raw materials since the steam creates passages (channels-tunnels) and it cannot process all the material completely, with steam distillation (Fig.3) for distilleries over 300 liters volume, are mounted a grid-diffusers (31) into (8)(Fig. 4, 5 and 6) to separating of raw material; for second and third levels steam is supplied from a steam generator (Fig. 3) through pipe (23); separated from raw material saturated steam with essential oils from first and second level is moved through pipes (29 and 30) to top of boiler (8) over the raw material in thirdly level; with grid-diffusers (31) reduces expenditure of steam for percentage of oil extracted.

*pressure in the hemisphere (52) is equal to zero .fwdarw. water left from (53) .fwdarw. t° = 95°C
*full power of cooling .fwdarw. water left from (53) .fwdarw. t° = 40-60°C
* .fwdarw. see DIVISIONAL APPLICATION (2) T° CA 02421141 DIVISIONAL APPLICATION (1) TO CA 0,242,1141

3. The device of claims 1 ~ 2, by dividing grids (31) in the boiler (8) (Fig.

4) through pipe (23) with cocks (24 and 25) is fed steam from steam generator (Fig. 3) for every one of separated levels;
through pipes (29 and 30) with cocks (27 and 28) passed saturated steam with essential oils at the top of the boiler (8) under the lid (42) (Fig.8 and 9), through pipes (45) and (44) with cocks (56, 57 and 58) steam passed from (8) into (52) and is directed to cooler (77) (Fig.12-1); in various combinations of closing or opening of cocks (24, 25, 27, 28, 56, 57 and 58) can be accurately adjusted pressure or vacuum, appropriate temperature for processing raw material total for the whole boiler (8) or explicit levels with material separated by grids (31); where (31) do not used, for water distillation (Fig.1) and steam distillation using cohobation device (Fig.18), the cocks (24,25,27 and 28) are closed.

4. The device of claim 1, cohobatin device to distill of material in liquid condition or distillate from previous distillations (144 and 145)(Fig.18) superheated steam heats the liquid in it gradually and increase a pressure into (8) causes a steam to pass through the space between the (144) and (145), get to the bottom, changes its direction vertically upwards and passes through the liquid;
when is opened the cocks (56.57 and 58) (Fig.8 and 9) in process of speed cooling on steam, under (42) over liquid in (144) is formed vacuum helping of steam to pass vertically through all the liquid before the liquid to begin boiling; passing through the liquid vapor entrained with her oil drops; with increase of time temperature of liquid grows gradually, means the liquid is treated consistently in the *first and second phase zones and after boil in third phase zone.

5. The device of claim 1, water jacket (53) (Fig. 8) increases the path of cooling but reduces the time for this as helps for gradual drop in temperature cooling of steam with small temperature differences when steam passing across the hemisphere (52) in direction (77)(Fig.12-1), this helps the condensation of steam is separated oil to a larger diameter drops; (53) helping when necessary to provide new water for steam generator (Fig. 3) or in boiling water generator (Fig. 1) the water is already heated to the maximum temperature.

6. The device of claim 5, water jacket (53) can be replaced with bent pipe with form of spiral as the water outlet from cock (47) is beginning with the narrowest diameter of the spiral, the input water comes from (77) to a cock (50) is the end of the spiral with largest diameter thereof, that facilitates the construction of the structure.

*first and second phase zones and after boil in third phase zone .fwdarw. see DESCRIPTION