• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a device for extracting the assets of a product, comprising: a. a tank (110) sealed; b. means (111, 112) for filling the tank with the product to be treated and a solvent; vs. an agitator (140); d. a hydraulic circuit, comprising: di. a duct (151) for sucking the contents (190) of the tank; dii. a hydraulic pump (150) whose suction is in hydraulic communication with the suction duct (151); diii. a discharge duct (153) connected to the discharge of the pump (150) and to the tank (110) having a section (154), said processing section, made of a material transparent to the microwave; e. a device comprising a magnetron (160) and a waveguide (161) adapted to subject the action of the microwaves the contents of the section (154) of treatment of the discharge tube. The invention also relates to a method for implementing this device
    公开号:FR3032892A1
    申请号:FR1600074
    申请日:2016-01-14
    公开日:2016-08-26
    发明作者:Francois Barbier
    申请人:Erpim；
    IPC主号:
    专利说明:

    [0001] The invention relates to a device and a method for the assisted extraction of the asset of a product. The invention is particularly, but not exclusively, intended for the industrial extraction of an essential oil, or more generally for the extraction of an active ingredient from products, in particular plants. The extraction methods are based on the difference in solubility of the compounds present in a mixture and in a solvent. The invention is more particularly directed to the case of a solid mixture, that is to say more particularly, a plant. The extraction techniques known from the prior art include: extraction by hydrodistillation; 10 - extraction by Soxhlet; extraction, called batch mode using solvent mixtures; extraction by sonication; - microwave assisted extraction; extraction by supercritical fluid.
    [0002] These methods of the prior art all have limitations. Thus, extraction processes assisted by microwaves lead to high temperatures, likely to degrade all or part of the active ingredients whose extraction is targeted, including antioxidants. In addition, these processes require for their implementation that the treated product contains water, which interacts with the microwaves 20 to produce the extraction. Also these methods of the prior art using microwaves are not suitable for treating dry or dehydrated products without prior hydration. Ultrasonic processes lose effectiveness depending on the nature of the plants used. In addition, the product manufacturers are seeking more environmentally friendly methods, and as such wish to limit the use of extraction methods using hydrocarbon solvents such as Hexane (C6H14 isomers). . The invention aims to solve the disadvantages of the prior art and for this purpose concerns a device of the asset of a product, which device comprises: a. a sealed tank; B. means for filling the tank with the product to be treated and a solvent; vs. an agitator acting inside the vessel; 3032892 2 d. a hydraulic circuit, said circulation circuit, comprising: di. a suction line for the contents of the tank, preferably at the bottom of the tank; dii. a hydraulic pump whose suction is in hydraulic communication with the suction duct; diii. a discharge pipe connected to the discharge of the pump and to the tank, preferably at the top of said tank, and having a section, said processing section, made of a material transparent to the microwave; e. a device comprising a magnetron and a waveguide capable of subjecting the contents of the treatment section of the discharge tube to the action of microwaves. Thus the device of the invention combines the action of the solvent and microwaves microwaves being applied to the outside of the tank, in a reduced portion of the conduit which allows to dispense a homogeneous exposure of the product contained in the microwave channel, according to single-mode exposure, and a finer regulation of the exposure intensity so as to preserve the product's assets. In addition, the control of the exposure to microwaves is regulated and controlled throughout the process by the flow rate imposed on the product in the treatment section, so that the process which is the subject of the invention is both more efficient and effective. faster in the extraction of the asset and controlled more finely, for the preservation of quality of the asset, in comparison with the processes of the prior art. The microwaves acting on a section of the circulation duct, the treatment of the product by these microwaves is possible without difficulty even if the volume of the tank is very important, which opens the application of micro-assisted extraction. to large volume processing. The circulation of the mixture during the treatment combined with the action of the agitator, allows a cohobation and ensures a high yield of the extraction. "Assets" of a product means a substance such as an odoriferous, medicinal, cosmetic, coloring or energetic substance without this list being exhaustive, which substance is contained in a product, generally, but not exclusively, vegetable . By way of nonlimiting examples, the process and the device which are the subject of the invention are advantageously used to extract iris butter from 3032892 3 iris rhizomes, fungicides for the vine from ginger, supplements foodstuffs from crushed vine shoots, antioxidants for cosmetic applications from grape must, oils scented from blends of sunflower oil with other ingredients such as peppers or ginger. They are also suitable for treating dehydrated products such as rose berries, peppers, lavender, coffee, tea or cocoa, or wood such as sandalwood. The invention is advantageously implemented according to the embodiments described below which are to be considered individually or in any technically operative combination. According to a first embodiment of the device which is the subject of the invention, the vessel comprises a double wall and said device comprises: f. means for the circulation of a coolant between the walls of said double jacket.
    [0003] This embodiment makes it possible to precisely regulate, by heating or cooling, the temperature in the tank. The combination of the regulation of the temperature and the flow rate of the product makes it possible in particular to concentrate the action of the microwaves on the core of the fibers of the product without causing a cumulative heating over the entire contents of the tank.
    [0004] Advantageously, the device according to the invention comprises: g. means for regulating the pressure in the tank. Thus the extraction is assisted either by pressurization or by the evacuation of the vessel, depending on the nature of the product and the extracted asset. For this purpose, the pressure regulating means advantageously comprise a vacuum pump.
    [0005] Advantageously, the device which is the subject of the invention comprises: h. means for recovering and treating the vaporized solute in the tank. Thus, the means for pressurizing and controlling the temperature cooperate, independently of the microwave power applied to control the evaporation of the solute in the tank. Advantageously, the device object of the invention compotes: i. means for weighing the tank.
    [0006] Thus, the treatment conditions are adaptable depending on the volume treated and the amount of solute recovered. Advantageously, the discharge pipe comprises a bypass and a valve for emptying the tank. Thus the circulation means of the solute are advantageously used for the emptying of the tank which also makes it possible to complete the cleaning of the device during the passage from one type of product to another. Advantageously, the device according to the invention comprises: j. a sonotrode adapted to subject the contents of the tank to an ultrasonic vibration 10 Thus the mechanical action of the ultrasonic waves is combined with the other effects of temperature, pressure, microwaves and solvent to complete the extraction of the asset. The invention also relates to a method using a device according to the invention for extracting the active ingredient from a product, which process comprises the steps of: i. fill the tank with the product and a solvent; ii. circulating the contents of the tank by means of the circulation circuit by submitting said contents to the microwaves in the treatment section, for a duration adapted to the product; Iii. recovering the solute comprising the active agent and the solvent; iv. separating the active agent from the solvent; v. Thus, the method of the invention allows the extraction of a large variety of assets from a wide variety of products under optimum conditions by controlling the various process parameters of the process. According to exemplary embodiments, the solvent is water, an oil or an alcohol. Thus, the method which is the subject of the invention, according to the chosen solvent, whose efficiency is enhanced by the action of microwaves, allows extraction particularly respectful of the environment or to favor the efficiency of the extraction.
    [0007] Advantageously, the method which is the subject of the invention comprises, before step iii) the steps of: vi. pre-soaking the product with the solvent at a pressure lower than the atmospheric pressure between steps i) and ii) vii. modify the pressure inside the tank during the steps following step vi). Advantageously, the method which is the subject of the invention comprises, before step iii), a step consisting in: viii. regulate the temperature in the tank by means of the circulation of the coolant. Advantageously, the method which is the subject of the invention comprises, before step iii), a step consisting in: ix. subject the contents of the tank to an ultrasonic vibratory stress. Advantageously, the method which is the subject of the invention comprises, before or after any one of steps i) to v), a step consisting in: x. weigh the contents of the tank. These different embodiments make it possible to better control the conditions for extracting the active ingredient and to improve the efficiency of the process. They are advantageously combined. According to a particular embodiment, the device which is the subject of the invention comprises: means for directly exposing the contents of the microwaves tank according to a multimode exposure; I. a bottom agitator. This embodiment makes it possible to expose the product directly in the tank, which, in certain circumstances, is preferable, especially for the treatment of fragile products such as iris rice.
    [0008] The invention is explained below according to its preferred embodiments, which are in no way limitative, and with reference to FIGS. 1 and 2, in which: FIG. 1 represents in a schematic diagram an exemplary embodiment of the device which is the subject of the invention; and FIG. 2 illustrates, in a schematic diagram, an alternative embodiment of the device of FIG. 1, making it possible to directly apply the microwaves inside the tank, and in which the installations common with those of Figure 1 have not been shown.
    [0009] FIG. 1, according to an exemplary embodiment, the device which is the subject of the invention comprises a tank (110), for example, said tank is made of a stainless steel. This tank comprises, according to this embodiment, a hatch (111) adapted to be closed in a sealed manner to introduce the product to be treated inside the tank. By way of nonlimiting examples, the product is a plant product, such as fruits, a herb, flowers, barks, for example, dried iris rhizomes, powdered ginger, shredded vine shoots, grape must, desmodium, sunflower oil, rosemary, peppers, or mixtures of these products. A conduit (112) opening into the vessel (110) allows a solvent to be introduced into said vessel. By way of example, the solvent is distilled water, an oxygenated organic solvent such as an alcohol or an ester, an aromatic hydrocarbon or haliphatic organic solvent or a halogenated organic solvent without this list being exhaustive. Advantageously, the process and the device which are the subject of the invention make it possible to use water as a solvent for many extraction cases. Thus, the method which is the subject of the invention comprises a first step of filling the tank (110) with a mixture (190) comprising the product to be treated and a solvent. The solvent is chosen according to the product and the asset to be extracted as well as the relative proportions of product and solvent. The device according to the invention advantageously comprises safety devices (not shown) adapted to explosive atmospheres, according to the type of solvent provided. The volume of the tank is adapted, for a given installation, according to the volume of the batches to be treated. According to this embodiment, the portion of the vessel containing the product is provided with a double wall (113) and a device (120) for circulating a coolant in this double wall. Thus, this device (120) 25 is used to heat, by indirect heating, or to cool as much as necessary the contents (190) of the tank (110). According to this exemplary embodiment, a duct (131) opening into the tank (110) is connected to a vacuum pump (130) and thus makes it possible to put the inside of the tank under a partial vacuum, the suction being regulated by a valve (132) placed on said suction duct (131). According to this embodiment, a de-oiler (133) is used to recover the condensed vapors in the tank prior to discharging the sucked air. Advantageously, this device for modifying the pressure in the tank is adapted to create a partial vacuum as well as an overpressure. A conduit (134) provided with a valve (135) makes it possible to put the inside of the tank at atmospheric pressure, to allow the hatch (111) to be opened. Thus, according to an exemplary embodiment of the process which is the subject of the invention, after filling the vessel with the product to be treated and the solvent, the pressure is lowered inside the vessel from 500 to 950 mbar. to reach a minimum absolute pressure of the order of 63 mbar (6.3.103 Pa) to promote the pre-imbibition of the product with the solvent. According to an exemplary embodiment, this pre-imbibition step preceding the microwave treatment is continued for a period of time in 2 hours and 3 hours. It is particularly useful in the case of treating a dry product such as ginger powder or cumin with an aqueous solvent. A stirring device (140) ensures a stirring of the contents (190) of the tank during the entire treatment. Since the tank is not subjected to the action of microwaves, according to this embodiment, the presence of this stirrer does not present any risk of creating arcs or plasma inside said tank. According to this exemplary embodiment, one or more sonotrodes (170) make it possible to subject the contents (190) of the tank to ultrasonic vibrations, and to add a sonication effect to the combined extraction process by the solvent and the microwaves. Unlike the known solutions of the prior art, the microwaves 20 do not act directly inside the tank, which allows the device which is the subject of the invention to produce a homogeneous treatment of the whole of the tank. contained by mircoondes even if the volume of the tank is important. For this purpose, a circulation device is connected, here at the bottom of the tank, by a suction pipe (151). Said duct (151) is connected to the suction of a pump (150). According to an exemplary embodiment, the pump (150) is a pump capable of sucking a viscous liquid comprising solid particles. The suction flow rate of the pump (150) is regulated by the speed of the drive motor of said pump, and the opening of the suction valve (152). According to an exemplary embodiment, this flow rate is controlled variable or constant during the extraction process. This valve (152) suction 30 also isolates the pump of the contents (190) of the tank during filling operations. The discharge of the pump (150) is connected to a discharge duct (153) which returns product sucked into the tank (110). In its path, the discharge duct 3032892 8 (153) passes through a magnetron (160) capable of generating microwaves at a frequency of the order of 2.4 Ghz, preferably of the order of 915 MHz for powers. greater than 10 KW. Alternatively, other frequencies are usable, depending on the nature of the product treated, but the frequency of 2.4 Ghz is suitable for the treatment of all natural products, as the frequency of 915 Mhz is for the high powers . Said discharge duct (153) consists, for example, of a stainless steel, except for the portion (154) passing through the magnetron (160) and subjected to microwaves, which is made of a material transparent to mirrors for example a ceramic or a plastic material. A waveguide (161) serves to concentrate the action of the generated microwaves to said portion (154). Thus, when the magnetron (160) generates microwaves, the product circulating in this portion (154) of the discharge conduit is subjected to the action of said microwaves for a time which depends on the imposed flow rate. Microwaves excite the sensitive material molecules at the frequency used, more particularly water, and produce a heating of the material by creating a temperature gradient, in which the temperature is higher in the core of the fibers migrating heat outwardly, driving the active outward of said fibers where it is recovered by the solvent. Thus, this circulation achieves a cohobation. By way of non-limiting example, the co-approval rate is of the order of 10 lites / minute (1.67 × 10 -4 m 3 s -1). The treatment is continued until the desired extraction rate, the maximum extraction rate being a function of the product treated and generally included in the mass of between 0.2 per 1000, for example for iris butter, and 2 per cent , for example for the essential oil of ginger. Typically this treatment is continued for a duration up to 8 hours and subjecting the product-solute mixture to a microwave power of between 30 kW and 75 kW at the magnetron, without this example of implementation being limiting. . The pressure and the temperature in the tank are controlled during the treatment, typically between room temperature and 110 ° C for the temperature and between -950 mbar and 2 bar relative to the pressure, in order to control evaporation of the solute.
    [0010] It is pointed out that although represented as manually operated valves, all the valves of the device of the invention are alternately controlled valves so that the treatment is automated.
    [0011] Controlled raising of the temperature inside the vessel, typically to a temperature of between 100 ° C and 110 ° C, causes vaporization of the solute. The vapor is collected in a chimney (180) placed for this purpose at the top of the tank, then it is directed to a circuit (181, partially shown) of treatment 5 where it is condensed and where the active ingredient is separated from the solvent and purified by methods known from the prior art such as the Florentine vase or by evaporation. The residues present in the tank are drained, for example by means of a duct (158) bypassing the discharge duct (153) and a drain valve (157). This emptying device is also used for rinsing the installation.
    [0012] According to this exemplary embodiment, the device that is the subject of the invention comprises a weighing device (191). As an exemplary embodiment, the tank (110) is suspended in a support (not shown) by calibrated springs whose deformation is measured to determine the variation of the weight of said tank during the treatment process. Alternatively, the tank (110) rests on a support (not shown) 15 from which it is spaced along a short stroke by means of jacks provided with a force sensor, for example a piezoelectric sensor. This weighing device makes it possible to adapt the treatment conditions, in particular the pressure, temperature, co-approval flow rate and treatment time, as a function of the quantity treated and the quantity of solute recovered.
    [0013] 2, according to a particular embodiment, the device according to the invention comprises means (260, 261) for directly applying microwaves in the tank (110). Said means comprise a magnetron (260) with a power of between 30 KW and 200 KW, at a frequency of 915 Mhz, and a waveguide (261) conveying the microwaves produced by said magnetron up to the inside. of the tank. This mode of exposure of the product to the microwaves is alternatively usable to that described in the previous embodiment, for example for the treatment of certain fragile products, simultaneously or in alternating cycles with the mode of exposure described with reference to FIG. Figure 1. The tank then behaves as a resonant enclosure achieving a multimode exposure of the product. In order to ensure a homogeneous exposure of the product contained in said tank (110) a tank bottom mixer (240) makes it possible to stir said product during its exposure. Said mixer is advantageously made of a dielectric material for its part located 3032892 10 inside the tank to avoid any creation of arcs or sparks. Thus exposed directly to microwaves, the tank (110) has it vis-à-vis the product it contains as a still. The active ingredient vaporizes under the action of heat and the vapor is recovered by the stack of the tank and directed by a circuit (281) 5 appropriate to a condensing coil (not shown). Thus the device object of the invention allows to use alone or in combination different extraction techniques and is thus versatile. The foregoing description and the exemplary embodiments show that the invention achieves the desired objectives, in particular, it makes it possible to treat by a combination of the effect of the solvent and the microwaves a large quantity of product and allows, by the combined action of different extraction assistants to use environmentally friendly solvents while maintaining industrial yields and production rates.
    权利要求:
    Claims (17)
    [0001]
    REVENDICATIONS1. Device for extracting the assets of a product, characterized in that it comprises: a. a tank (110) sealed; b. means (111, 112) for filling the tank with the product to be treated and a solvent; vs. an agitator (140) acting inside the vessel; d. a hydraulic circuit, said circulation circuit, comprising: di. a duct (151) for sucking the contents (190) of the tank, preferably at the bottom of the tank; dii. a hydraulic pump (150) whose suction is in hydraulic communication with the suction duct (151); diii. a delivery duct (153) connected to the discharge of the pump (150) and to the tank (110), preferably at the top of said tank, and having a section (154), called the treatment section, made of a transparent material in the microwave ; e. a device comprising a magnetron (160) and a waveguide (161) adapted to subject the action of the microwaves the contents of the section (154) of treatment of the discharge tube.
    [0002]
    2. Device according to claim 1, wherein the vessel (110) comprises a double envelope (113) and which comprises: f. means (120) for the circulation of a coolant between the walls of said jacket;
    [0003]
    3. Device according to claim 1, comprising: g. means (130, 131 132) for regulating the pressure in the vessel (110).
    [0004]
    4. Device according to claim 2, wherein the pressure regulating means 3032892 12 comprises a vacuum pump (130).
    [0005]
    5. Device according to claim 2, comprising: h. means (180, 181) for recovering and treating the vaporized solute in the tank (110). 5
    [0006]
    6. Device according to claim 1, comprising: i. means for weighing the tank.
    [0007]
    7. Device according to claim 1, wherein the discharge duct (153) comprises a bypass (158) and a valve (157) for emptying the tank. 10
    [0008]
    8. Device according to claim 1, comprising: j. a sonotrode (170) able to subject the contents of the tank to an ultrasonic vibration.
    [0009]
    9. Method, implementing a device according to claim 1 for extracting the asset of a product, characterized in that it comprises the steps of: i. filling the tank (110) with the product and a solvent; ii. circulating the contents (190) of the vessel through the circulation circuit by subjecting said contents to the microwaves in the treatment section (154) for a period appropriate to the product; iii. recovering the solute comprising the active agent and the solvent; iv. separating the active agent from the solvent; there. drain the residue from the tank.
    [0010]
    The process of claim 9 wherein the solvent is water. 25
    [0011]
    The method of claim 9, wherein the solvent is an alcohol.
    [0012]
    The process of claim 9 wherein the solvent is an oil.
    [0013]
    The method of claim 9, using a device according to claim 3, and comprising before step iii) the steps of: vi. pre-soak the product with the solvent at a pressure below atmospheric pressure between steps i) and ii) vii. modify the pressure inside the tank during the steps 5 following step vi)
    [0014]
    The method of claim 13, using a device according to claim 5, and comprising between steps ii) and iv) a step of: viii. regulate the temperature in the vessel by means of the circulation of the coolant so as to vaporize the solute.
    [0015]
    15. The method of claim 9, using a device according to claim 7, comprising before step iii) a step of: ix. subject the contents of the tank to an ultrasonic vibratory stress. 15
    [0016]
    The method of claim 1, using a device according to claim 6, comprising before or after any one of steps i) to y) a step of: x. weigh the contents of the tank.
    [0017]
    Device according to claim 1, comprising: 20 k. means (20, 261) for directly exposing the contents of the vessel (110) to the microwaves in a multimode exposure; I. a bottom agitator (240).
    类似技术:
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    同族专利:
    公开号 | 公开日
    FR3032892B1|2020-02-28|
    FR3032891A1|2016-08-26|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US20060153758A1|2005-01-12|2006-07-13|Vasco Cheung|Method and apparatus for the extraction of plant constituents|
    CN101020126A|2006-11-09|2007-08-22|温州市神华轻工机械有限公司|Continuously extracting pipeline type microwave equipment|
    WO2013170678A1|2012-05-15|2013-11-21|嵩县开拓者钼业有限公司|Industrial microwave ultrasonic reactor|
    FR3003181A1|2013-03-18|2014-09-19|Innovation & Dev Company Idco|METHOD AND INSTALLATION FOR EXTRACTING BIOLOGICAL PRODUCTS BY MICROWAVES|CN107982960A|2017-12-08|2018-05-04|中国科学院过程工程研究所|A kind of magnetic particle combination membrane extraction device and extracting process|
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    CN109224510A|2018-11-20|2019-01-18|那坡康正天然植物提取有限责任公司|A kind of extractor producing multitude's beans extract|
    CN109331498A|2018-11-20|2019-02-15|那坡康正天然植物提取有限责任公司|A kind of multi-function extractor|
    CN109331500B|2018-12-19|2020-12-15|涂乙芬|Surrounding type ultrasonic extraction device|
    法律状态:
    2017-01-27| PLFP| Fee payment|Year of fee payment: 2 |
    2017-12-29| PLSC| Publication of the preliminary search report|Effective date: 20171229 |
    2018-01-30| PLFP| Fee payment|Year of fee payment: 3 |
    2019-01-29| PLFP| Fee payment|Year of fee payment: 4 |
    2020-01-30| PLFP| Fee payment|Year of fee payment: 5 |
    2021-01-29| PLFP| Fee payment|Year of fee payment: 6 |
    2022-01-27| PLFP| Fee payment|Year of fee payment: 7 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1550290A|FR3032891A1|2015-01-14|2015-01-14|DEVICE AND METHOD FOR ASSISTED EXTRACTION OF PRODUCT ASSETS|
    FR1550290|2015-01-14|
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