DD216165A1 - METHOD AND DEVICE FOR OBTAINING ETHERIC OILS - Google Patents

Abstract

The invention relates to a method and a device for obtaining essential oils from vegetable products. The oils are particularly useful in the pharmaceutical, cosmetic and food industries. The aim of the invention is the improvement of the known container method and the increase in yield of essential oils. It is the object of the invention to develop a method in which a uniform container loading takes place and a device adapted thereto is used. According to the invention, the harvested plant is conveyed into an upwardly completely open second vehicle whose container-like loading space simultaneously forms part of the distillation vessel and which is filled by smaller spatial displacements in relation to the harvesting vehicle, the second vehicle is closed at rest with a stationary lid and closed at one Stationary plant the crop is subjected to a known steam distillation. The lid and container have sealing elements and the container has a steam fork arranged at the bottom and a lateral discharge flap. By the invention, a substantial increase in yield in the recovery of essential oils from a variety of plants or plant parts is possible.

Description

01153 DD

Method and device for obtaining essential oils

Field of application of the invention. '

The invention relates to a process and a device for obtaining essential oils from vegetable products. The ethereal oils are particularly useful in the pharmaceutical, cosmetic and food industries.

Known technical solutions

Several processes are suitable for the extraction of ethereal oils. The method of squeezing, subsequent solvent extraction and distilling off the solvent is meaningful only in plant species with extremely high oil contents. The extraction of the oils with the aid of solvents is technologically complicated and requires the subsequent liberation of the extraction product from solvent fractions. This is difficult to achieve in high quality at the relatively low boiling ranges of ethe ·· risehen oils.

On the other hand, steam distillation has proved to be the most suitable "method for obtaining ethereal oils having a high degree of purity". Discontinuous bubble distillation plants are known (Gildemeister ₉ Hoffmann, The Essential Oils, Berlin 1961, Volume ₉ VII, S _β 257-382),

Furthermore, from Landing American Essence, 1969, a Oontainerverfahren is known in which the harvested fresh drug is blown in eipaen provided with a hatch tractor semitrailer, and this'Transportbehälter is connected after filling to a stationary distillation plant "The De *» stillation is obviously from the unhitched hangers overhead at the highest point of the asymmetrical pyramid-shaped roof by means of live steam from the stationary steam

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Supply The roof with the lower part of the trailer forms a spring. The damping stations are designed so that several containers can be processed at the same time. The container size fluctuates between 2.0 to 6.0 t of prehicle receiving capacities. An emptying of the distillation residue eifölgt a tailgate of the saddled trailer ·

A disadvantage of this method is in particular that eii distillation chamber produces a conical, verfiizter structure of the distillation material by the blowing of the harvested plants in &, the SiOH also not changed, retire shaking, but rather yet solidified. Due to the asymmetric pyramid-shaped Daohauf construction, in which the Einfülluke is located on a short side of the pyramid, an asymmetric cone of the distillation material is formed, which is flowed through unevenly in the case of steam at the bottom of the steam vapor, which ultimately lead to losses in yield must, * is conceivable a mechanical VerteiluiEig within the distillery room * whereby however additional equipment expenditure is necessary ^ or an increased steam expenditure per produced kilogram oil, what the energy balance loaded *

Another disadvantage is that each einzeihe container must be designed as a closed container and the roof cap is not einzubär for several containers a working line ·. '.'. ;. :: ^ '. 'V * - ^{1 V:} -.' · '.' ^: '·

Aim of the Invention · ·; '.. ._ r. /: ''. ' , ^; '_;" ^: ..",

It is an object of the invention to improve the known Gontainerverfahren and in particular 'to increase' the yield of etherisehen oils · '' · ^-;.. '·''/' .. .. .. ·.. ';.;;;;;;;; • ·.

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Essence of the invention ; <

The invention is based on the task to develop a method in which a uniform container loading takes place and a device adapted thereto is used.

According to the invention, the process for recovering essential oils from vegetable products by steam distillation wherein the vehicle loaded with the crop is at the same time the distillation vessel is that the harvested plant is transported by the harvesting vehicle into a fully open second vehicle, the container-like one Cargo space at the same time a part of the distillation tank and its filling is done by slight spatial displacement in relation to the harvesting vehicle. The loaded second vehicle is then provided at rest with a steam-tight lid with Dampfaüslaß and the now closed container-like distillation tank connected to a stationary Dampfq.uelle, 'The steam then flows through a located at the bottom of the distillation, steam outlet openings provided with steam fork through the crop passing · The resulting mixture of steam and essential oils is steam at ausläß * ä ß & lid removed, supplied to a stationary cooler, condensed and collected in a collecting vessel. In this vessel, which is preferably constructed according to the principle of Florentine bottle, the separation takes place in oily and aqueous phase * The oily phase can continuously withdrawn laterally or discontinuously by pushing both phases in the narrowing neck of Auffangsg; efäßes and decrease the oily Phase to be deducted overhead

After completion of the distillation is a side flap of the ISestillationsraumesj. is on the open side of the steam fork, that is, on the side that faces

01153 UD 11

the leaking tine is open, and the distillation residue removed. This is preferably done by tilting the loading surface of the vehicle on which the dehumidifier is located. The fuel oil substantially completely freed from the essential oils thereby leaves the distillating space and can then be plowed under or economically used as a secondary raw material ,

It is preferred to subject the freshly harvested plant in coarsely chopped form, in particular with about 10 cm length of chop, the Bestil3ation, in particular to reduce the spaces between the JP plant eggs. As a result, a dense space filling adapted to the distillation and better steam utilization is possible.

A uniform filling of the container in the form of the second vehicle is facilitated if the second vehicle is a drawn parallel to the harvester trailer, record the speed of changes and lateral direction corrections the Ertitefzeug preferably blown shredded material at all points of its hold evenly to a desired level can. The filling level is expedient about two-thirds of the side wall height.

The second vehicle is according to the invention completely top-'pfeexif. The cargo space is preferably geometrically approximately an open cuboid, whose largest side surface is the open area *

The second vehicle can after loading to a, preferably located in the immediate vicinity of the harvested area, station ^ SinTichtuhg be approached, there provided with the lid of Destillatiohsbehälters and the steam supply via a mounted on the second vehicle steam connection with the stationary steam ore ** or.

01153 DD 11

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Steam supply system to be connected. There is also a connection from the steam outlet on the lid to a stationary cooler and a condensate and / or separating vessel. Although the system is open, pressure should be monitored in the distillation room for safety reasons to regulate the supply of steam or to take other appropriate measures in the event of a pressure increase.

The supplied amount of steam is not critical and should be designed so that an economic operation of the system results.

The condensed mixture of water and essential oil is fed to a separation vessel which preferably operates in the manner of the Florentine bottle. In this case, the water at the bottom of the vessel and the essential oil can be removed via a side drain or overhead ", the Kondensatzulauf occurs

· ·. · 'Ι

separately in the upper part of the vessel * The condensate temperature is preferably below 40 ° C. in order to obtain the complete spectrum of the essential oil.

> After completion of the distillation, the separation of the distillation vessel from the stationary part takes place by removing the stationary stationary lid or by dissolving the connection between Dampfwrasenschiauch and Deekel and subsequent removal of Deckelse It is the second vehicle preferably moved back to the Er'nntefläche, the De ~ The inclined position is achieved by hydraulic lifting of the container-like container on the second vehicle, which may preferably be a trailer. The distillation residue slips almost completely out of the container without mechanical aids out and this is then ready for re-loading «·

01153 DD 11

A quasi-continuous operation of the stationary distillation apparatus is obtained if there are several steam connections and several subsequent feeds to the cooler, to which it is possible to switch over when using a plurality of second vehicles with a distillation space.

The process according to the invention can in principle be used in all plants which supply essential oils. These include, in particular, peppermint, aniseed, dost, rosemary, lavender, sage, caraway, coriander, fenoeel, spruce and pine needles. Plants such as KÜmme ^ L, coriander and fennel can already be harvested as whole plants before their complete maturity because of their small fruits. If necessary, licked pieces of wood (chips) can be added to loosen up in the distillation room.

To these plants also spice plants, such as marjoram, thyme ,, onion, dill (or dill tips) tamrehsaatgut etc., in which the inventive Verf al also is particularly advantageous use.

Preferably, the content of essential oil in the dry plant is at least 0.5 ^. However, it may also be greater, for example in pine needles, if their oil is desired. This alone is an economic problem.

By the method according to the invention it is possible to obtain ethical oils in yields of 80 to more than 90 % of the theoretical yield. Durcb ^. the uniform loading of the distillation room with the harvested plant makes it possible to obtain a uniform flow of the steam within the liquor and to avoid loss of yield. The absence of Stahldekel of the container during loading substantially reduces the mass of the second vehicle and contributes to the saving of material, in particular of fuel.

.0115-3-DP It

The invention also relates to a device for carrying out the process. It is a device for obtaining essential oils from vegetable products by means of steam distillation, consisting of a stationary steam generation, cooling and separation plant and a mobile distillation vessel, the at the same time represents the laden with the Brute goods vehicle. Characteristic of the device is that the mobile distillation vessel is made of

a) an upwardly completely open, containment-type container on the loading surface of a vehicle, wherein the upper Sa ^ d of the container has sealing elements and at the bottom of the container with a Dampfaustrittsö'ffungen provided steam fork is arranged, the open side indicates the direction of discharge, and the

, container further comprises a discharge, located in the sealed flap, and. .

b) consists of a stationary, preferably at the also stationary Destiilationsanlage, mounted lid whose lower pand has sealing elements and which is provided with a steam outlet,

The bottom surface of the distillation vessel corresponds approximately to the floor area of the vehicle loading area «

The sealing elements of the container edge can from an open ^x upwards U "profile consists ^ which through its upper edge away filled with an elastic sealing material" Here, the sealing material should be selected so that, by its own pressure, the lid mass is not completely in the U- Profile is pushed in, but extends beyond the top edge of the U-profile. The sealing material is preferably sponge rubber. _β

The sealing elements of the lid can for example consist of a downwardly open U-profile, which is larger than the U-profile of the container edge and bell-like over

01153 DD 11

Preferably, the internal dimension of the cover U-profile is selected to be twice as large as the external dimension of the container to facilitate the fitting of the cover. The cover already closes by its own mass, but can preferably still be secured by additional closure elements ·

A steam fork is placed on the bottom of the distillation tank. It consists of an end-to-end, longitudinal tube from which several transverse tubes emerge in the form of tines. The cross tubes have Dampfaustrittsoffnungen, both axially and at the closed end horizontally, The openings (holes) are mounted approximately at equal intervals and alternately offset by 90 ° to achieve a uniform application of steam to the crop. The distance between the bottom and steam fork should be small, preferably about 5 cm, to facilitate the dumping of the residue. The lid is preferably of symmetrical conical, pyramidal construction and has a steam outlet at its highest point. The container is emptied via a flap mounted on the side of the container, preferably arranged in the lower two-thirds of a container wall and closed by closure elements, e.g. Screw knob, secured, Again, a seal is required. It is preferably boulder a laterally open U-! Profile, which is filled with an elastic sealing material, which in schlössenei? Flap pushes against the container wall everywhere ·

Condensate drain valves may be disposed above the bottom surface of the Behälteis, / and in the upper fiehälterteil a pressure gauge, the re- an overpressure which may occur can gistrieren '.

The invention will be explained in more detail by examples. In the accompanying drawing mean

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Pig. 1 front view of an embodiment of the second vehicle according to the invention

Fig. 2 side view of FIG. 1 with lifted lid

Fig. 3 steam fork>

Fig. 4 sealing lid / container

Figi 5 sealing flap / container \

embodiment

Peppermint is mown with a forage harvester, chopped and blown onto a second vehicle driving alongside. This consists of a train vehicle with Ήänger, on which a container-like distillation vessel 1 is mounted. The emptying flap 5 is closed. The container is evenly with the plant parts by the speed corrections Zugfehrzeugs and slight lateral training ^ soft thereof filled. The filling height is about 100 to 120 cm. After filling the trailer is fed to the stationary device. The container lid 2 located there is placed on the distillation container 1 after rough cleaning of the container rim (sealing material) and the lid closure elements 3 (eg bayonet caps) are actuated. The seal between the lid and container is made by the sealing material 22, which is located in the container U-profile §1 · The lid U-profile 20 presses against the sealing material. The steam flow line is connected to the steam outlet 6. The steam supply line to the steam inlet 7 is connected, the condensate drainage closed and opened the steam supply. The steam distributed over the steam fork 10 in the peppermint chop and the entrained ethereal oils pass through the steam outlet into a water-cooled condenser, where they are cooled to about 40 ° C., condensed and collected in a Florentine bottle attached thereto. · _,

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The Köhdensatabgang is adjusted so that the condensate ^ water level remains unchanged. The Pfeffermihzöl standing over the KondensatÄfasser can be continuously withdrawn through a located at this level lateral overflow (especially in quasi * continuous distillation of several Destillationsbehättern successively) or by raising the condensate water level after completion of the distillation and decrease of the oil on one of the top of the bottle located, separate outlet. There were about 0.5 to 0 * 7 nr / h steam with a pressure of about 2.0 to

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2.2 kp / cm used. The pressure in the distillation space is controlled via the manometer 11.

After completion of the distillation wiid the steam supply line between stationary plant and trailer was separated, the Kondensatwasserabiäß 9 opened, lifted the lid of the container via a traction device on the Deckelaufhänguhg 8 after opening the closure elements and gebeut the trailer for reloading back to the harvested area. By hydraulically lifting the loading area of the trailer on one side and thus tilting the distillation vessel, the distillation residue can slip out to the open side of the steam fork tines out 12 later sub-plowed or fed to the feeding. Optionally, the remainders of the residue are removed manually and also the sealing elements of the flap are cleaned. After closing the side flap, the drawer / distillation tank is ready for use again. .

The Kläppenabdichtung is such that a laterally open U-Pröf11 24, the sealing material located within the U-profile 26 presses against the container edge 25.

01153 DD 11

Example 1:

2 630 kg of "Multimentha" peppermint were evenly distributed in the DestiEatibnsraum. "The steam pressure was 1.9 - 2.0 kp / cm ² , the steam temperature about 100 ° C. After 40 minutes of steam injection" the Distillation for three hours "The condensate discharge was about 200 l / h at a condensate temperature of 40 ° C. At a leaf-stem ratio of the air-dry whole plant of 44:56, a yield of 4.61 l of peppermint oil was obtained as clear, yellowish oily liquid The analysis showed no residual oil as a loss in the distillation residue.

Example, 2:

The second cut of 2,080 kg used under the same conditions as in Example 1 gave, at a condensate temperature of 35 to 40 ° C., 5.72 l of peppermint oil, the leaf-to-leaf ratio being 40:60 first and second cut was 89 %. ...

Example 3:

, '. , 2 230 kg of peppermint "Polyhybrid-7 ^M (1st section) were distilled under the conditions mentioned in Example 2. 6.64 ml of peppermint oil were obtained as a clear, oil-oily liquid at a leaf-stem ratio of the air-dried granules of 55 ί 45.. '.

Example 4:

The second cut of 1020 kg according to Example 3 yielded 2,950 1 peppermint oil at a condensate discharge of 180 l / h and a condensate temperature of 38 ° C. The ilatt-stem ratio was 57:43.

01153 DD 11 12 -

Example 5:

2 470 kg of peppermint "Lekarsstvennaya mehtholnaya" gave after distillation at a condensate temperature of 4CM-5 ⁰ C 8j71 1 peppermint oil as a clear, yellowish, oily liquid with a leaf * stem ratio of 45 i 55. The etherisehe oil content of fresh whole plant was 1.62 ml / 100 g dry matter. The yield was 97.98 % compared to the theory *

Example 6:

2 600 kg of small-sized pine needle green material were introduced into the distillation tank. The distillation was carried out with Dam lf from 2.0 to 2.2 kp / cm ² and about 100 ° CV After two hours of distillation time to receive 1.9 1 Kiefernnädeiöl. The theoretical yield was 2.16 l / t, corresponding to 0.2 % of the Prischgutes. The practically achieved yield of pine seed oil of 0.79 l / t corresponds to only 34 % of the content of NaOH. After the distillation was stopped, the essential oil content of the distillation residue was still 0.03 ml / 100 g. ι

In variieruiig certain conditions, a substantial increase in yield can be achieved.

Example 7:

Käpillar-GrC studies of the MUItimertha oils obtained according to Example 1 with corresponding laboratory-obtained peppermint oils did not show any differences in the composition. The ethereal oil of Example 1 has a very high concentration of menthone both in container distillation and in laboratory experiments (57.65 % and 54.57 %, respectively). This leads to a lowering of the l-menthol content (25.37 % or 24.94 ^).

01153 DD 11

The causes of this significant shift in the ingredient spectrum could be an early harvest date as well as soil and currency conditions.

Claims (17)

01153 DD 11 .- 14 - Civil claim A process for the production of essential oils from vegetable products luitters Wasserdämpdestillatiöh, said. The laden laden with the crop vehicle at the same time the distillation vessel, characterized in that the harvested plant is transported by the harvesting vehicle in an upwardly completely open second vehicle, the contäinerarii cargo space zugleioh a 3 represents ile the distillation vessel and its filling takes place by slight spatial displacements in relation to the harvesting vehicle, which is provided in boot position with a steam-tight lid with steam outlet, the second vehicle is connected to a stationary steam source and via an am Steam is passed through the crop at the bottom of this vehicle located in Destillstionsraum steam fork, wherein the formed steam / oil mixture cooled in a known manner via a connected to Dampfaüslaß the lid stationary cooler and con is condensed, the entrained oil separated in a likewise known manner, and the second vehicle after completion of the distillation utid opening a side flap of the distillation space a'n the open side of the steam fork is freed from the distillation residue *. ^:; '' V. '.'.-' .. ·. ' · ·. ^; -. ' 2. The method according to item 1, characterized in that the harvested plant is present in chopped form. 3o method according to item 2, characterized in that the shredding length of the plant is about 10 cm. 01153 DD - 15 - 4, method according to item 1, characterized in that the second vehicle is a drawn parallel to the harvesting vehicle trailer. 5 «Procedure according to point 1 _? characterized in that the second vehicle at the location of its largest cross sections? is open to the top. 6. The method according to item 1, characterized in that the "Level in the loading / distillation room" is about two-thirds of the page height.     #. . 7. The method according to item 1, characterized ^ ^ that the harvested area is in the field of stationary equipment. 8. The method according to item 1, characterized in that the emptying, the distillation residue is carried out by tilting the loading / DestiUationsraumes. 9. Move η to point 8, characterized in that the inclination is made to the longitudinal side. 10 * Method according to item 1, characterized in that the distillate is separated via a device according to the principle of the Florentine bottle. 11. The method according to item 1, characterized in that the Eondensattemperatur is below 40 ° C. 12. The method according to item 1, characterized in that the plant from the group peppermint, fennel, anise, Dost, 01153 DD 11 - 16 - Hosarin and lavender · was considered · 13 * Method according to item 1, characterized in that the plant is selected from the group of the spice plants, preferably marjoram, thyme, dill, onion, carrot seed. 14 · Procedure according to item 12 *, characterized in that the plant is peppermint. 15. The method according to item 1, characterized in that it is the plant to pine · * and / or spruce needles. 16. The method according to item 12 and 14, characterized in that the content ah ethereal oil in the air-dry plant mass is at least 0.5 % * 17 * Device for obtaining essential oils from vegetable products by means of steam distillation, consisting of a stationary Dampferzeugüngs-, KUhI and separation plant and a mobile distillation vessel, which is at the same time with dom crop beiaaehö vehicle, characterized in that the mobile distillation vessel a) an upwardly completely open, container-like container on the back of a vehicle, wherein the upper edge of the container has sealing elements and at the bottom of the container provided with Dampfaustrittsoffnungen steam fork is arranged, the open side is directed to the Sntladungsseite and the container further in the discharge direction, has sealed flap, and 01153 DD 11 b) consists of a stationary, preferably at the also stationary distillation plant, mounted lid whose lower edge has sealing elements and which is provided with a Dämpfauslaß. 18. Device according to item 17, characterized in that the bottom surface of the distillation vessel corresponds approximately to the base area of the vehicle loading surface. 19 · Device according to item 17, characterized in that the sealing elements of the container edge consist of an upwardly open U-profile, which filled over its upper edge away with an elastic sealing material '. is. .. ... '. , 20. The device according to item 19, characterized in that the sealing material is chosen so that it still protrudes beyond the U-profile top in compression by the applied lid. _ 21. The device according to item 17, characterized in that the sealing elements of the lid consist of a downwardly open U-profile whose inner dimension is greater than the outer dimension of the sealing elements of the container edge. 22. The device according to item 21, characterized in that the inner dimension of the lid U-profile is about twice as large as the outer dimension of the container U-profile. Device according to item 17, characterized in that the steam fork is a pipe system in which a longitudinally closed, longitudinally extending pipe ' several go also at the end closed cross tubes go tinkenfö'm. _ 01153 DD 11 ^'':.:. '' -'18'-. ·.; .- ^.: '-...:: 24 * Preliminary drying according to item 17, characterized by the fact that the steam fork is located only a short distance from the container bottom. 25; Provision according to item 24, characterized in that the distance is about 5 cm. I 26. Vorriöhtung according to item 17, characterized in that the steam fork has in the tines achsiäle Däfflpfaustrittsbohrühgen. 27 »Device according to item 26, characterized in that the holes are alternately offset at equal intervals. 28 * Preparation according to item 23, characterized in that the transverse tube has a steam outlet bore at the closed end. 29. Device according to item 17, characterized in that the flap seal takes place via a laterally open Ü-profile, the elastic Dichtüngsmateriai located therein presses against the container edge. Preparation according to item 17, characterized in that the flap is secured in the lower two thirds of the container wall by means of closure elements. 31 * device according to item 17, characterized by the fact that the Cover secured by additional closure elements '' is * "'·"' ', ·'. . '. 01153 DD 11 32. Device according to item 17, characterized in that the lid, conically upwards at the same angle, tapers and is arranged at its highest point of the steam outlet. - Hierau 3 pages drawings