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Title:
A METHOD FOR EXTRACTING VEGETABLE OILS AND A COUNTERFLOW DEVICE FOR PERFORMING SAID METHOD
Document Type and Number:
WIPO Patent Application WO/2005/100518
Kind Code:
A1
Abstract:
The invention relates to an oil and fat industry, in particular, to production of vegetable oils by a method of extraction by organic solvents. Aim of the invention is to provide such method of the vegetable oils extraction, such device for its implementation, and such extractor of a submersible type being a part of the device, which allow to increase intensity of mass exchange at the extraction stage, to increase concentration and purity of produced miscella, providing heightening output of the extracted oil and improving its quality, and also to obtain defatted meal suitable for further processing. For achieving these aims, the process is carried out at a temperature of phase transformation 'fluid-vapor' in conditions of cavitation and intensive mixing of the solvent in non-mixed surrounding of a solid phase of the material under extraction, and solvent vapors, which are produced in this process, are removed, condensed and returned back into the process, providing the re-circulation of the solvent.

Inventors:
KUSNETSOV VITALY NIKOLAEVICH (RU)
Application Number:
PCT/RU2005/000165
Publication Date:
October 27, 2005
Filing Date:
April 04, 2005
Export Citation:
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Assignee:
STAVRULOV IGOR ANATOLIEVICH (RU)
KUSNETSOV VITALY NIKOLAEVICH (RU)
International Classes:
C11B1/10; (IPC1-7): C11B1/10
Domestic Patent References:
WO2003060044A12003-07-24
Foreign References:
US4453832A1984-06-12
US2074988A1937-03-23
US1862945A1932-06-14
US2334015A1943-11-09
RU2166533C22001-05-10
Attorney, Agent or Firm:
Tsetovich, Natalie Leonidovna (50-1-24 Moscow, 2, RU)
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Claims:
WHATIS CLAIMED IS:
1. A method of vegetable oils extraction by organic solvents, including a loading of a material to be extracted, an extraction of the oil by the solvent in a counter flow extractor of a submersible type, a collection of the solvent vapors, their condensation and return into a process, a meal and a miscella removal, characterized in that the extraction process is carried out at a temperature of a phase transformation "fluid vapor" in cavitation conditions.
2. A device for vegetable oils extraction by organic solvents, containing a loading Column with a socket for entering a material to be extracted, sockets for entering tlie worked out air with the solvent vapors, and for removal of the purified air, a dosing screw, a condenser, a counter flow extractor of a submersible type with sockets for removal of the solvent vapors from the extractor into the condenser and for return of the condensed vapors, a unit for heating the meal, and sockets for the solvent input and the miscella output, characterized in that the counter flow extractor of a submersible type is provided by heating elements for maintaining a temperature of phase transformation "fluidvapor" inside, it is made in the form of one or several sections, and a decanter having a widening to the bottom loading tube intended to create a. gas seal is positioned before the first section of the counter flow extractor.
3. T he d evice according to e laim 2 , c haracterized i n t hat t he c ounter flow e xtractor sections are positioned with an inclination to the side of loading of the material to be extracted.
4. The device according to claim 2, characterized in that the first, by way of the material motion, section of the counter flow extractor is made inclined, and the next one is made horizontal.
5. The device according to claims 3, 4, characterized in that the unit for the meal heating is positioned in the upper part of the last, by way of the material motion, section of the counter flow extractor.
6. A counter flow extractor of a submersible type for vegetable oils extraction by organic solvents according to claim 1, characterized in that it contains a body with a socket for input of a material to be extracted, a socket for input of a solvent, sockets for output of solvent vapors, a miscella and a meal, it fitted with heating elements for maintaining inside a temperature of phase transformation "fluid vapor", and it is made in the form of one or several sections.
Description:
A METHOD FOR EXTRACTING VEGETABLE OILS AND A COUNTERFLOW DEVICE FOR PERFORMING SAID METHOD

This invention relates to the oil and fat industry and, in particular, to production of vegetable oils by a method of extraction by means of organic solvents. Methods of vegetable oils production by means of cold or hot pressing are known and widely spread at present time. Maximal amount of oil can be extracted by the hot pressing; nevertheless, such oil contains many concomitant substances. Extraction of seeds in cold presses gives a lesser amount of corresponding oil, but the oil contains less concomitant substances. All oils produced by means of pressing, contain a big amount of admixtures and require some purification. Extraction of vegetable oils by volatile organic solvents (often by benzene low-boiling fractions) and subsequent distillation of the solvent relates to chemical methods. There are known methods of vegetable raw stuff extraction with a help of organic solvents, which methods provide a treatment of the raw stuff prepared for the extraction by solvent vapors, then a preliminary extraction of the oil in a counter flow with the solvent, by means of repeated sprinkling of the extracted material by a miscella, and completing the extraction process in a vertical column sprinkled by the miscella. Distillation of the solvent from the extracted material is provided by an action of overheated vapors of the solvent that are not leaving the device but, condensing on the meal, come back in the extraction process (see Russian patent No. 2,166,533, CI lB 1/10, 1999). Device according to this patent includes: a loading column with sockets of inputs of the material under extraction and the purified gas and air mixture, and of outputs of the purified air; a traverse unit with a unit of miscella re-circulation, and a vertical extraction column with a screw inside and sockets for inputs of the materal under extraction and the overheated vapors of the solvent, and of output of the meal. The vertical extraction column for this process is made counter flow. The main drawback of this method and device for its implementation, and of the extractor itself, is a low velocity of the mass exchange in the extraction process, which requires rather high proportion of the solvent - the material under extraction and results in obtaining of the miscellas of low concentration. The known methods of vegetable oil extraction includes a loading of a material to be extracted, an extraction of the oil by a solvent in a counter flow extractor of a submersible type, an extraction of the solvent vapors, their condensation and return to the process, offtake of the meal and the miscella. The material to be extracted is impregnated with the saturated vapors of the organic solvent before the extraction. Extraction of the oil by the solvent is carried out in the counter flow extractor of a submersible type and in a vertical counter flow extractor. Extraction of the solvent vapors, their condensation and return to the extraction process is provided in the process. The extraction of the solvent from the worked-out meal is carried out by means of influencing on it by overheated solvent vapors and heating the meal in the discharge zone. (See Russian patent No. 2,210,589, Cl IB 1/10, 2001.) The device for the implementation of the known method is also known. It contains a feeding column with a socket of input for material to be extracted, sockets of input for worked-out air with vapors of the solvent, and of output for the purified air; a dosing screw; a condenser; a counter flow extractor of a submersible type with sockets of output for solvent vapors from the extractor into the condenser and of return for condensed vapors; a unit for heating the meal; and sockets of input the solvent and of output the miscella from the device. The counter flow extractor of a submersible type, a part of the device, is placed in a horizontal position. These method, device and extractor are the most close to the proposed ones. Main disadvantage of this method, the device for its implementation and, accordingly, the extractor, as well as of previous ones, is a low mass exchange intensity in the extraction process, caused by a relatively low (45-50 0C) temperature of the process. Besides, the cooling of the materal under extraction by sprinkling it with the solvent, which is provided in the device, results in obtaining the meal with increased oil content; and the use of the pump for miscella re-circulation makes difficult its exploitation conditions (because of existence in the miscella of a big amount of particles with high abrasive properties) leads to the existence of mechanical admixtures in the taken off miscella. Aim of this invention is to provide such method of a vegetable oils extraction, such device for its implementation, and such counter flow extractor of a submersible type that is a part of the device, which could allow to increase intensity of mass exchange on the extraction stage, to increase concentration and purity of the obtained miscella, providing increase of the extracted oil output and improvement of its quality, and also to obtain the defatted meal of a rather high quality suitable for further processing. This aim is achieved, due to the fact that in the known method of vegetable oil i

extraction of organic solvents, which includes a loading of a material to be extracted, an extraction of the oil by a solvent in a counter flow extractor of a submersible type, an offtake of the solvent vapors, their condensation and return to the process, extraction of the meal and the miscella, the extraction process is carried out at the temperature of the phase transformation "fluid-vapor" in cavitation conditions. To achieve this aim with the known d evice for the extraction o f v egetable o ils b y organic solvents, which contains a feeding column with a socket of input for material to be extracted, sockets of input for worked-out air with vapors of the solvent, and of output for the purified air; a dosing screw; a condenser; a counter flow extractor of a submersible type with sockets of output for solvent vapors from the extractor into the condenser and of return of condensed vapors; a unit for heating the meal; and sockets of input of the solvent and of output of the miscella, the counter flow extractor of a submersible type is provided by heating elements for maintaining inside the extractor the phase transformation "fluid-vapor" temperature. The extractor is made in the form of one or several sections, and a decanter is placed before the first section of the extractor, said decanter has a loading tube enlarging downwards to make a gas seal. The sections of the counter flow extractor of a submersible type can be made horizontal, inclined, vertical, or combined. An optimal design of the device for the extraction of vegetable oils provides for inclination of each section of the counter flow extractor of a submersible type to the side of loading of the material under extraction. Another implementation of the counter flow extractor of a submersible type provides for making the first on the way of material under extraction section inclined, and making the next one horizontal. The counter flow extractor of a submersible type for the extraction of vegetable oils by organic solvents contains, for achieving the aforementioned aim, a case with sockets of input for material to be extracted, for a solvent, and of output for vapors of the solvent, the miscella and the meal; it contains also heating elements for maintaining inside the extractor the temperature of a phase transformation "fluid- vapor"; it is made in the form of one or several sections. Numerous investigations of the inventor made a base for this invention. They confirmed the fact that the optimal temperature for the process of extraction of vegetable oils by organic solvents is the temperature of boiling of the solvent at a pressure corresponding to the pressure in the extractor, for example, this temperature lies in intervals of 68-72 0C for solvent "Nephras". The oil extraction at such temperature is carried out in conditions of the phase transformation "fluid-vapor" and is accompanied "by cavitation processes caused by the solvent boiling and by extensive agitation of extractable substance in the layer of material under extraction. Hydrodynamics of the process is such, that each particle of the layer of the no agitated material is strongly and repeatedly washed by the extracting substance. All this leads to the drastic increase of the heat and mass exchange and, accordingly, to the intensification of the extraction process. The proposed method is implemented, and the device and the counter flow reactor work, as follows: A material to be extracted enters into a loading column where it is impregnated with saturated vapors of a solvent that come therein together with worked-out air. Then the material is transferred into decanter by means of a dosing screw, purifies from crude admixtures the miscella, which comes by counter flow. Then it comes upon a counter flow extractor of a submersible type, which sections are fitted with heating elements. The extraction process is carried out at the temperature of the phase transfoimation "fluid-vapor" in conditions of cavitations. The resultant solvent vapors are removed from the extractor and are condensed. The condensate with a temperature near to the boiling temperature is returned into extractor, providing, by this way, the solvent re-circulation. This allows to decrease supplying into the device of a fresh solvent and, accordingly, to increase concentration of the finished miscella. Completeness of the oil extraction is such, that practically defatted meal reaches the last section of the counter flow extractor, where the solvent is taken off by means of feeding of overheated solvent vapors and heating the meal itself. Example of realization of the method is given below, which shall not be considered as any limitation of the invention. The material to be extracted in the form of soybean flakes enters the loading column where it is impregnated by saturated vapors of the solvent that enter there together with the worked-out air, Then it is moved, by means of the dosing screw, into the decanter, purifying the miscella that enters by counter flow from the rough admixtures. Afterwards it enters the counter flow extractor of a submersible type. Six sections of this extractor are inclined to the loading side and are furnished with heating elements. The heating elements are made in the form of vapor-jackets; they maintain temperature of 68-72 0C inside the sections. The extraction process is carried out in conditions of phase transformation "fluid-vapor" and cavitation. The produced solvent vapors are removed from the extractor sections and are condensed; the condensate with temperature near to the toiling one is returned to the last (on the way of the extracted material) section of the extractor, providing, by this way, the solvent re-circulation. The meal, entering the last, seventh, section of the counter flow extractor for the final extraction and distillation of the solvent, has oil content of 0.7-1.0 %. Extraction time is 21 minute. Concentration of the final miscella is up to 50-70 %. The essence of the invention is explained by drawings, where Fig. 1 represents a general view of the device for vegetable oils extraction, including the counter flow extractor of a submersible type, and Fig. 2 represents one of its embodiments. The device for extraction of vegetable oils includes loading column 1 with socket 2 for entering the material to be extracted, socket 3 for entering the worked-out air with the solvent vapors, socket 4 for removal the purified air, dosing screw 5 providing a stable level in the loading column 1 of the material to be extracted, decanter 6 serving for a preliminary purification of the miscella from rough admixtures and for maintaining of the constant level of the extracting substance in the extractor of a submersible type. The counter flow extractor of a submersible type is made in the form of several inclined sections 7, 8, 9, 10, 11, 12, connected each other by means of overload units 13, 14, 15, 16, 17. Each of the inclined sections 7, 8, 9, 10, 11, 12 have screws 18 positioned inside the sections for transportation of the material to be extracted, and heating elements, made, for example, in the form of vapor-jackets 19. Each of the inclined sections 7, 8, 9, 10, 11, 12 is provided by sockets 20, 21, 22, 23, 24, 25 for removal of the solvent vapors that are produced in the course of extraction, through drop catchers 26, 27, 28, 29, 30, 31 into condenser 32, and by sockets 33, 34, 35, 36, 37, 38 for return the miscella into the sections in case of itschurning. The last section of the counter flow extractor is made in the form of inclined column 39 with a screw inside (not shown in the drawing). Inclined column 39 is furnished with socket 40 for removal of the solvent vapors from it into condenser 41; by socket 42 for return a condensate from condensers 32 and 41; by socket 43 for replenishment the extractor by the solvent from the reversing system. The inclined column 39 has also socket 44 for unloading the meal from the device, unit 45 placed in the upper part of the column for heating the meal, and chute 46 for the inclined column 39 evacuations in case of necessity. Decanter 6 is provided by socket 47 for the miscella output from the device. Socket 47 position determines the miscella level in the inclined sections 7, 8, 9, 10, 11, 12, 39. Loading tube 48, broadening to the lower part, is positioned inside decanter 6. The material under extraction coming from dosing screw 5 descends through this tube. The tube serves to form a gas seal preventing passage of the saturated solvent vapors from decanter 6 into loading column 1. Socket 49 is placed in the upper part of decanter 6. This socket connects a gas space of the decanter 6 with a gas space of the inclined sections (not shown on the drawings). Sockets 50, 51, 52, 53, 54, 55 are placed in the lower part of each inclined section 7, 8, 9, 10, 11, 12; the sockets serve for the evacuation of the sections in case of necessity. Fig. 2 s hows a d evice v ariant, w hich c ontains 1 oading c olumn 56 w ith s ocket 57 for lead-in the material to be extracted, socket 58 for lead-in of the worked-out air with the solvent vapors, socket 59 for output of the purified air, dosing screw 60, decanter 61, the extractor of a submersible type having inclined 62 and horizontal 63 sections with placed inside them screws 64 and 65 accordingly, which are fitted with heating elements in the form of vapor-jackets 66 and 67 accordingly. The counter flow extractor of a submersible type has another one vertical section 68 for the oil final extraction; screw 69 is placed inside this section, and a heating element in the form of vapor-jacket 70 is placed outside this section. The upper part of section 68 has socket 71 for unloading the meal and unit 72 for heating the meal, and the lower part has socket 73 for deflection the solvent vapors into condenser 74 and socket 75 for return of condensed vapors, socket 76 for replenishment the extractor with the solvent, and socket 77 for evacuation of section 68. Socket 78 is provided for evacuation of inclined section 62 and decanter 61. Decanter 61 is furnished with socket 79 for the miscella output from the device. Loading tube 80 broadening to the lower part is positioned inside decanter 61; it serves to form a gas seal preventing passage of the solvent saturated vapors from decanter 61 into loading column 56. The material under extraction coming from dosing screw 60 descends through this tube. Socket 81 is placed in the upper part of decanter 61 connecting the gaseous space of the decanter with the gaseous space of section 63 (not shown in the drawing). The device and its part, the counter flow extractor of a submersible type, according to Fig. 1, work as follows. The material prepared for extraction comes through socket 2 into loading column 1. Then, dosing screw 5 transfers it into loading tube 48 of decanter 6, where it comes through the miscella layer, is saturated by the miscella and clears itself from the air, which comes through socket 49 into the gaseous space of the inclined sections. The material, saturated by the miscella and cleared from air, goes down into inclined section 7 and is removed by a screw (not shown in the drawing) into section 8 through transferring unit 13. The material, in the process of transfer, reaches the zone of boiling miscella and saturates it with the oil. This process is repeated in inclined sections 8, 9, 10, 11, 12 of the counter flow extractor o f a s ubmersible t ype. T he m iscella s trength ( content o f t he o il i n t he s olvent) i s growing at each next inclines section, and the content of the oil in hard particles of the material to be extracted is decreased. This content is 1-1.5 % at the output of section 12. The pure solvent in inclined section 39 washes the material. Then, a screw (not shown in the drawing) transports the material from the zone of deepening in the solvent into the zone of the solvent vaporizing. The extracted material cleared from the solvent is unloaded through socket 44. The solvent vapors generated at the miscella boiling in sections 7, 8, 9, 1 0, 11, 12, move through drop catchers 26, 27, 28, 29, 30, 31, are purified from a foam and drops entrained by the vapors, are condensed in condenser 32. The solvent vapors produced at the solvent evaporation in section 39, are condensed in condenser 41. A condensate of the solvent vapors is poured out through socket 42 into section 39 and moves in the direction of the decanter t hrough i nclined s ections 1 2, 1 1, 1 0, 9 , 8 , and 7 t owards t he f low o f t he m aterial under extraction. The solvent from the recycling system is fed through socket 43 into section 39 to replenish the extractor in amount corresponding to its content in the miscella obtained, which is moved out from the extractor through socket 47 of the decanter 6. The vapor-air mixture is transported by additional units from condensers 32 and 41 through socket 3 into loading column 1, is purified from the solvent vapors (by means of absorption of the solvent by the oil contained in the material to be extracted) and removed through socket 4. The device and the counter flow extractor according to Fig. 2 work as follows. The material prepared for extraction comes through socket 57 into loading column 56. Then, dosing screw 60 transfers it into loading tube 80 of decanter 61, where it comes through the miscella layer, is saturated by the miscella and clears itself from the air, which comes through socket 81 into the gaseous space of section 68. The material, saturated by the miscella and cleared from air, goes down into inclined section 62 and is removed by screw 64 into horizontal section 63 of the counter flow extractor. The material, in the process of transfer, reaches the zone of boiling miscella saturating it by the oil. The pure solvent washes the material in vertical section 68 of the counter flow extractor. Then the material is transported from the zone of submersion into the solvent to the zone of the solvent evaporation. The material being extracted and cleared from the solvent is unloaded through socket 71. The solvent vapors that are formed as a result of the miscella boiling in sections 62, 63 of the counter flow extractor, and in section 68, are condensed in condensation unit 74. The condensate of the solvent vapor is poured out through socket 75 into section 68 and moved in the direction of the decanter through horizontal 63 and inclined 62 sections of the counter flow extractor towards the flow of the material under extraction. The solvent is fed through socket 76 to section 68 for replenishment of the extractor from the re-circulating system in amount that corresponds to content of the solvent in the obtained miscella that is removed from the extractor through socket 19 of decanter 61. The vapor-air mixture is transported by means of additional devices from condenser 74 into loading column 56 through socket 58, cleared from the solvent vapors (absorption of the solvent by the oil contained in the material under extraction), and removed through socket 59. The applicant's investigations confirmed that the optimal temperature for the extraction process of the vegetable oils by the organic solvents is a temperature equal to the temperature of the solvent boiling at a pressure corresponding to the pressure in the extractor. These investigations show that at this temperature the oil extraction occurs in conditions of phase transformation "fluid-vapor", accompanied by cavitations processes, conditioned by the solvent boiling and extensive mixing of the extracting substance in the layer of the material to be e xtracted. H ydrodynamics o f t his p rocess i s s uch t hat e ach p article o f t he 1 ayer o f n on- mixing material is intensively and many times washed by the extracting substance. AU this leads to the sharp increase of the heat and mass exchange and, accordingly, to the intensification of the extraction process. By this way, the present invention allows to increase the intensity of the mass exchange on the extraction stage, to increase the concentration and purity of the miscella obtained, to provide increase in output of extracting oil and improvement of its quality, and also to receive the defatted meal of high quality.