FORM 2
THE PATENTS ACT 1970
(39 of 1970)
&
The Patent Rules 2005
PROVISIONAL SPECIFICATION
(see sections 10 & rule 13)
1. TITLE OF THE INVENTION
COMPACTED UPFLOW SOLID LIQUID EXTRACTOR AND ITS APPLICATIONS

2. APPLICANT (S)
"NAME

NATIONALITY

ADDRESS

a) Almet Corporation Limited

Indian

332, Adhyaru Industrial Estate, Sun Mill Compound, Lower Parel, Mumbai-400 013. India

b) Lali Arvind Mallinath

Indian

Chemical Engineering Department
Institute of Chemical Technology,
University of Mumbai, Nathalal Parikh
Marg, Matunga ( East),
Mumbai-400 019
Maharashtra
India

3. PREAMBLE TO THE DESCRIPTION
PROVISIONAL SPECIFICATION
The following specification describes the invention.
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Field of Invention
The present disclosure relates to a solid-liquid extractor, more specifically an extractor arrangement specially suited for efficient extraction of non-volatile and/or volatile extractive products from natural sources.
Background of the invention
The extraction of valuable active principles from natural sources using simple and efficient extraction system is an important required attribute towards the development of new therapeutic and agricultural products. The present invention of extractor systems is useful to extract high value substances from natural bioresearches such as crustacean shells, seaweed, agricultural crops, wild and modified plants. The present invention is applicable in the pharmaceutical, perfumery and cosmetics, food and food processing, bio-technological and chemical industries for the extraction of valuable extractive products from the said solid materials.
DE 3,318,317 discloses a process and an apparatus in which the still undamaged, that is not yet disintegrated product and the extraction liquid are, separately, subjected to an elevated gas or air pressure. The extraction liquid, after a predetermined time of action, is brought into contact with the product with the pressure being maintained. The pressure is then suddenly relaxed, the cells of the products are destroyed and the aroma substances or the like being liberated, which are then taken up directly by the extraction liquid and after a predetermined time of action and, if required, with mechanical filtration, are led off without loss.
RU 2,045,981 (CI) discloses a continuous extractor for solid body liquid system for extraction of organic products. The system has two units for charging raw material
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and extractant, each having hermetically sealed body and rotor with circumferentially positioned receptacles for charging liquid and solid materials.
RU 2,091,120 (CI) discloses extractor for solid liquid system, which includes vertical cylindrical housing with technological branch pipes and thermostating jacket. Extractor is also provided with baffles mounted over periphery and agitator mounted co-axially in housing with elliptic filter element secured onto it co-axially; filter element separates extract collecting chamber in its lower portion.
US 5,776,317 discloses extractor for soxhlet solid liquid extraction, consisting of extraction vessel to which reflux line is molded in one piece. Solvent is vaporized in a heatable distillation vessel and routed via a steam line into an extraction vessel located above the distillation vessel. The extraction vessel is provided to hold the material to be extracted and the extract and is made with a cooler for condensing the solvent or extractant.
WO 83/02571 discloses an extractor for the liquid solid extraction of extractive materials from natural substances comprising a support frame hinged about an axis parallel to a fitting floor and arranged in housing. It consists of rotary devices of different types acting on the extraction mass, such as suction, agitation and coating devices. The devices are capable or rotating about an axis perpendicular to the fitting floor.
The references incorporated herein disclose the extractor system with stirring or agitating devices, or with the heating of extractant liquid so as to extract the active principle/s from the solids. None of the prior art discloses an extractor system wherein the solid materials from which the extractive substances to be extracted, is pressed or compacted by a means of a perforated plate having a projections to achieve better solid liquid contact. Also none of the system discloses the extraction of the active principles by operating an extractor with upflow of extracting liquid
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giving high efficiency. Therefore, there is a need to develop an extraction device for the extraction of active principles from the solid material in a simple and efficient manner.
Brief description of the Drawings
The features, objects and advantages will be evident from the following description of the preferred embodiments of the present disclosure taken in conjunction with the accompanying drawing in which; Figure 1 is a schematic illustration of the apparatus and method of the invention.
1: Cylindrical column,
2: Inlet to feed solid material,
3: Screw shaft,
4: Perforated plate,
5: Projections attached to perforated plate,
6: Solid material,
7: Flow distributor,
8: Inlet located at the bottom side of the extractor,
9: liquid outlet,
10: Top column sealing plate,
11: Drive (manual, motorized or hydraulic),
12: Leak proof joint,
13: Condenser,
14: Solid material entry point,
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15: Hinge or hinge like arrangement,
16: Supporting plate,
17: Outlet (for vapors, gas or volatile matter),
18: Lid for solid inlet and
19, 20 and 21: Valves
Description of the Invention
Accordingly, it is an object of the present disclosure to provide a solid liquid extractor system for efficient solid liquid contact and interaction, more specifically an extractor for extraction of active principles from natural sources (for example, but not limited to, plant(s), herb(s), shrub(s), sea weeds, animals, insects etc.).
Another object of the present disclosure is to provide the application of such extractor and the process for the extraction of active principles from said natural sources.
Broadly, the present disclosure relates to an extractor system comprising a vertical vessel or column, a means to feed the solids (natural materials) into the extractor adjacent to the first (top) end of the extractor, and a means to compact or pack the fed solid material into the extractor. The system used for compacting or packing of the solid materials into the extractor consists of a plate, preferably perforated and with downward projections, and is operated through a screw type shaft that can move up or down either manually or through motorized drive or hydraulic system. The extracting liquid enters into the extractor through an inlet located at the second end (bottom end) of the extractor and passes through a How distributor, which distributes the liquid evenly in to the extractor, extracts the said active principles from the said
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solid material/s, and is taken out from the outlet adjacent to the first end of the extractor. The residual liquid remaining inside the extractor after complete extraction is removed by a hot air or steam passed into the extractor and is collected through the second outlet adjacent to the first end of the extractor via a condenser system attached to the said second outlet. The solids packed in the extractor after complete extractions are removed from the bottom of the extractor, wherein the bottom plate and distributor are opened manually or through a motorized system.
Referring to Figure 1, in one of the embodiments of the present disclosure the extractor is composed of a cylindrical column 1 in which a flow distributor 7 is incorporated at the bottom end to distribute the incoming liquid or gas or steam evenly in to the extractor column. The solid material for extraction 14 is fed through inlet 2 located near the top of the extractor. The solid matter is fed in one lot, or many lots, and compacted by moving the slowly rotating perforated plate 4, provided with projections 5, the movement carried out through a screw shaft 3 and a drive (manual, motorized or hydraulic) 11. The perforated plate 4 with projections 5 performs multiple functions such as compacting and/or crushing the solid material, leveling of solid material, and allows the passage of extracting liquid through perforations without allowing solid material to leave the extractor. The compaction or packing of said solid material using the perforated plate 4 with projections 5 leads to good contact of said extracting fluid with said solid material 6, an hence good efficiency. The screw shaft 3 operates through a leak proof joint 12 held in place by top column sealing plate 10 and allows the screw shaft to rotate freely. The extracting liquid enters into the extractor column through inlet 8 and passes in upward direction through distributor 7 held in position by a supporting plate 16. The said extracting liquid extracts the active principle from the said solid material 6 while moving in upward direction and is taken out through the outlet 9 located towards first end of the extractor. The extracting liquid is either continuously passed through the extractor till the complete exhaustion of said solid material in the active content,
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or is re-circulated for complete extraction of said active principles from the said solid material, and is then displaced by fresh liquid. The residual extracting liquid is removed from the extractor by passing steam or air (preferably hot air or gas) through bottom inlet 8 and collecting the solvent as a condensate from condenser 13 attached to the outlet 17 adjacent to the first end of the extractor. While removing the residual extracting liquid as discussed above, the solid inlet 2 is closed using a lid 18. Alternatively, if a gas or steam is being used as extractant, it is passed upwards with solid inlet 2 closed, and the vapor passed through the condenser 13. The extracted or exhausted solid material is removed from the bottom of the extractor, by opening the bottom plate 16 which is moved manually through a hinge or hinge like arrangement 15, or is opened using motorized drive mechanism.
In another embodiment, the solid material is naturally occurring or modified materials such as but not limited to plant(s), herb(s), shrub(s), sea weeds, animals or insects.
In still another embodiment, the active principles extracted using the extractor of the present disclosure is primary or secondary metabolite.
In yet another embodiment the active principles extracted using the extractor of the present disclosure is non-volatile or volatile matter.
In one another embodiment the active principles extracted using the extractor of the present disclosure is therapeutic product; intermediate for the production of therapeutic product; has agricultural value such as insecticide, growth regulator; has cosmetic value such as flavor/perfumes.
In another embodiment the active principles extracted using the extractor of the present disclosure is protein(s), peptide(s) and/or nucleic acid(s).
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In another embodiment the active principles extracted using the extractor of the present disclosure is known molecule in the natural sources; is expressed or over expressed in the said natural sources or in any part of these natural sources by genetic manipulation/engineering or other methods known to those skilled in art.
In another embodiment the extractor of the present disclosure is used for extraction of active principles from any known natural sources or improved varieties of known natural sources, genetically manipulated/engineered natural sources, transgenics, derived via plant or animal cell culture and hybrid varieties of known natural sources.
In another embodiment the extractor of the present disclosure is used for extraction of single or multiple product(s) of interest from said natural sources.
In another embodiment the extractor of the present disclosure is used for extraction of single or multiple product(s) of interest from sources in pure or impure form. When the product of interest is extracted in impure form, it is further processed by known techniques such as chromatography, liquid-liquid extraction, crystallization to make it substantially pure for necessary application(s).
In another embodiment the extractor of the present disclosure is used for extraction of active principles from animals or part of animals, insects, or any other known solid material containing known said active principles.
In another embodiment for the extraction of active principles using the extractor, extractant can be a liquid, air, pure gas, or steam. The liquids can be polar solvent(s), non-polar solvent(s), ionic liquid(s) or mixtures thereof where as gaseous extractant can be supercritical carbon dioxide.
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Thus the potential applications of the disclosure is believed to be suitable to include but not limited to the extraction of ionic, non-ionic, zweitter-ionic active principles, intermediates, metals or mixture thereof useful for human, veterinary or agricultural applications from modified or unmodified natural sources. Therefore, the present disclosure can be easily applied to an industrial scale.
The following is the example carried out to demonstrate the extraction of artemisinin from Artemisia annua leaves using the solid-liquid extractor.. However the present disclosure should not be construed as limited to the description of the example.
Example 1
In the arrangement shown in Figure 1 a cylindrical column 1 (30 cm x 200 cm) provided with distributor 7, the solid material inlet 2, perforated plate 4, projections 5, screw shaft 3, top column sealing plate 10, liquid inlet 8, supporting plate 16, liquid outlet 9, outlet 17, and lid 18 is constructed from stainless steel (SS316). The solid material inlet 2 is positioned at 5 cm below the first end of extractor; where as the liquid outlet 9 is located 5 cm below the solid material inlet 2. The screw shaft 3 is operated manually. A SS316 condenser assembly 13 is attached to the outlet 17 located 2 cm below the top end of the extractor. Teflon pipe is used for connecting bottom liquid inlet to pump and liquid outlet to receiver. The extractor was used for extraction of artemisinin from Artemisia annua leaves used as solid feed. Table 1 shows results obtained on the invented extractor for the extraction of artemisinin from Artemisia annua leaves.
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Table 1: Summary of the parameters and results of artemisinin extraction using Compacted Upflow Solid Liquid Extractor (CUSLE)
Parameter Result
Artemisinin concentration in solid feed (% w/w) 0.26
Extractant flow rate (ml/min) 150
Quantity of solids (herbage) (Kg) 10
Total solvent volume used (Lit) 200
Artemisinin in extract (gm) 25.2
Artemisinin recovered (%) 96.9
10 Kg leaves of herb Artemisia annua were charged to the extractor through solid material inlet 2 and compacted by manually moving down the perforated plate 4 with projections 5. The extracting liquid (hexane) was pumped through the extractor at 150 ml/min flow rate in upward direction using a diaphragm pump. The extract containing artemisinin and other products was collected through the liquid outlet 9. After complete extraction, the residual extracting liquid form the herbage was removed by passing steam through the bottom inlet, and collecting the condensate from the condenser 13. Exhausted plant material was removed from the bottom of the extractor. The operation gave 96.9% artemisinin extraction from the leaves due to efficient contact of extractant with solid material (leaves) in the extractor.
Dated 3nd Day of April 2007

To
The Controller of Patents,
Patent Office at Mumbai
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