RO130896A0 - Continuous flow reactor for microwave- and ultrasound-assisted extraction of biologically active compounds from plants - Google Patents
Continuous flow reactor for microwave- and ultrasound-assisted extraction of biologically active compounds from plants Download PDFInfo
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- RO130896A0 RO130896A0 ROA201500035A RO201500035A RO130896A0 RO 130896 A0 RO130896 A0 RO 130896A0 RO A201500035 A ROA201500035 A RO A201500035A RO 201500035 A RO201500035 A RO 201500035A RO 130896 A0 RO130896 A0 RO 130896A0
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 11
- 238000000874 microwave-assisted extraction Methods 0.000 title claims abstract description 10
- 238000002137 ultrasound extraction Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 239000000341 volatile oil Substances 0.000 claims abstract description 13
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 8
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 229930002877 anthocyanin Natural products 0.000 claims abstract description 6
- 235000010208 anthocyanin Nutrition 0.000 claims abstract description 6
- 239000004410 anthocyanin Substances 0.000 claims abstract description 6
- 150000004636 anthocyanins Chemical class 0.000 claims abstract description 6
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 6
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000010685 fatty oil Substances 0.000 claims abstract description 4
- 239000013543 active substance Substances 0.000 claims abstract 4
- RXHIKAIVEMAPRU-JRIGQVHBSA-N sequiterpene Chemical class C1=C(C)[C@@H](OC(C)=O)[C@H](O)[C@@]2(O)[C@H](C)CC[C@@H](C(C)=C)[C@H]21 RXHIKAIVEMAPRU-JRIGQVHBSA-N 0.000 claims abstract 2
- 150000003505 terpenes Chemical class 0.000 claims abstract 2
- 235000007586 terpenes Nutrition 0.000 claims abstract 2
- 238000000605 extraction Methods 0.000 claims description 33
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 239000002023 wood Substances 0.000 claims description 3
- 235000013399 edible fruits Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- -1 flowers Substances 0.000 claims 1
- 238000009827 uniform distribution Methods 0.000 claims 1
- 239000012620 biological material Substances 0.000 abstract description 16
- 238000001914 filtration Methods 0.000 abstract description 4
- 235000018102 proteins Nutrition 0.000 abstract description 4
- 238000005119 centrifugation Methods 0.000 abstract description 2
- 230000001143 conditioned effect Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 238000004108 freeze drying Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000005445 natural material Substances 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000011877 solvent mixture Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 240000007049 Juglans regia Species 0.000 description 2
- 235000009496 Juglans regia Nutrition 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 235000001537 Ribes X gardonianum Nutrition 0.000 description 1
- 235000001535 Ribes X utile Nutrition 0.000 description 1
- 235000001466 Ribes nigrum Nutrition 0.000 description 1
- 241001312569 Ribes nigrum Species 0.000 description 1
- 235000016919 Ribes petraeum Nutrition 0.000 description 1
- 244000281247 Ribes rubrum Species 0.000 description 1
- 235000002355 Ribes spicatum Nutrition 0.000 description 1
- 241001529742 Rosmarinus Species 0.000 description 1
- 241001530490 Salvia rosmarinus Species 0.000 description 1
- 238000010795 Steam Flooding Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000015639 rosmarinus officinalis Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/11—Natural spices, flavouring agents or condiments; Extracts thereof obtained by solvent extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0211—Solvent extraction of solids in combination with an electric or magnetic field
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Acoustics & Sound (AREA)
- Physics & Mathematics (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Fats And Perfumes (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
Description
Reactor continuu pentru extracția asistată de microunde și ultrasunete a compușilor biologic activi din planteContinuous reactor for microwave and ultrasonic assisted extraction of biologically active compounds from plants
1. Descrierea brevetului1. Description of the patent
Invenția se referă la un nou tip de design de reactor chimic continuu cu microunde (MW) și ultrasunete (US), utilizate simultan la obținerea compușilor biologic activi din plante.The invention relates to a new type of continuous chemical microwave (MW) and ultrasonic (US) chemical reactor design, used simultaneously to obtain biologically active compounds from plants.
Sunt cunoscute în literatură mai multe metode de fabricare a uleiurilor esențiale din material biologic, printr-o varietate de mecanisme și configurații de echipamente. Astfel, cererile de brevet EP 1439218 A1, EP 1618798 A1, EP 1629725 B1, US 5002784 descriu procedee de extracție a uleiurilor volatile din diferite tipuri de materiale vegetale și echipamente asistate de microunde aferente procedeelor descrise.Several methods of manufacturing essential oils from biological material, through a variety of mechanisms and equipment configurations, are known in the literature. Thus, patent applications EP 1439218 A1, EP 1618798 A1, EP 1629725 B1, US 5002784 describe processes for the extraction of volatile oils from various types of plant materials and microwave-assisted equipment related to the described processes.
De asemenea, brevetul EP 1439218 A1 descrie un aparat de extracție cu microunde a compușilor volatili din material biologic, printr-un procedeu de hidrodistilare. Acest sistem îmbunătățește zona de condensare și răcire a vaporilor de apă din afara cavității de microunde.EP 1439218 A1 also describes an apparatus for microwave extraction of volatile compounds from biological material by a hydrodistillation process. This system improves the condensation and cooling area of water vapor outside the microwave cavity.
O metodă de extracție a uleiurilor volatile din material biologic ce cuprinde un aparat cu următoarele componente: o cavitate de microunde, cu o zonă de primire a microundelor, ce permite crearea unei presiuni scăzute în zona de microunde și camera de condensare.care sunt conectate printr-un tub, este descrisă în brevetul de invenție EP 1618798 A1.A method of extracting volatile oils from biological material comprising an apparatus with the following components: a microwave cavity, with a microwave receiving area, which allows the creation of a low pressure in the microwave area and the condensing chamber.which are connected by -a tube, is described in patent EP 1618798 A1.
O altă metodă de extracție a substanțelor volatile, cu solubilitate scăzută în apă este descrisă în brevetul EP 1629725 B1. Metoda așa cum este prezentată cuprinde următoarele etape:Another method of extracting volatile substances with low water solubility is described in EP 1629725 B1. The method as presented comprises the following steps:
1) Introducerea materialului biologic fără solvent în cavitatea de microunde;1) Introduction of solvent-free biological material into the microwave cavity;
2) Iradierea materialului biologic până când se elimină în totalitate substanțele naturale de interes;2) Irradiation of the biological material until the natural substances of interest are completely eliminated;
3) Transportarea substanțelor naturale prin convecția din zona de microunde în zona de răcire;3) Transportation of natural substances by convection from the microwave area to the cooling area;
4) Răcirea substanțelor naturale;4) Cooling of natural substances;
λ- 2 Ο 1 5 - - 0 0 0 3 5 ι s -οι- ansλ- 2 Ο 1 5 - - 0 0 0 3 5 ι s -οι- ans
5) Transportarea substanțelor naturale din zona de condensare în zona de colectare.5) Transportation of natural substances from the condensation area to the collection area.
Apa care transportă substanțele naturale, se întoarce parțial în zona de microunde printr - un sistem de scurgere.Water that transports natural substances is partially returned to the microwave area through a drainage system.
într - o etapă secundară substanțele naturale sau cele mai puțin solubile în apă sunt separate într - un solvent hidrofobic. Vaporii de apă sunt generați în interiorul cavității de microunde din amestecul apă/material biologic.in a secondary stage the natural or least water soluble substances are separated in a hydrophobic solvent. Water vapor is generated inside the microwave cavity in the water / biological material mixture.
O altă invenție, US 5002784 relatează o nouă metodă de extracție selectivă a compușilor naturali din material biologic crud, care necesită o scurtă perioadă de timp pentru extracție și utilizează un aplicator de microunde. Această metodă respectă toate principiile extracției convenționale, dar comparativ cu aceasta randamentele de extracție sunt mult mai bune. Operațiile de separare și purificare ulterioare necesită cerințe speciale.Another invention, US 5002784 relates to a new method for the selective extraction of natural compounds from raw biological material, which requires a short period of time for extraction and uses a microwave applicator. This method follows all the principles of conventional extraction, but compared to this the extraction yields are much better. Subsequent separation and purification operations require special requirements.
Noul sistem de extracție este alcătuit dintr-o cavitate de microunde multimod sau monomod și un sonotrod în care este introdus un reactor cu design specificat Reactorul este conectat la un sistem de antrenare cu vapori tip Clevenger sau Vas Florentin, pentru colectarea și separarea uleiului volatil, așa cum se prezintă în figura 1.The new extraction system consists of a multi-mode or single-mode microwave cavity and a sonotrode into which a reactor with a specified design is inserted. The reactor is connected to a Clevenger or Florentine vessel steam drive system for collecting and separating volatile oil, as shown in Figure 1.
Figura 1. Reactor continuu pentru extracția asistată de microunde și ultrasunete a compușilor biologic activi din plante ^-2815--00035t 9-01-2015Figure 1. Continuous reactor for microwave and ultrasonic assisted extraction of biologically active compounds from plants ^ -2815--00035t 9-01-2015
Procedeul conform invenției prezintă numeroase avantaje: masa de material biologic prelucrată per șarjă este de minim 100 ori mai mare decât în procedeul discontinuu, se evită fenomenul de spumare a materialului biologic și implicit evenimentele nedorite, randamentul de extracție a substanțelor naturale crește cu până la minim 25%, se reduce semnificativ timpul de extracție, se obține un produs de o puritate ridicată și o calitate superioară din punct de vedere al compoziției chimice în comparație cu alte metode și sisteme de extracție în câmp de microunde și/sau metode neconvenționale, cum ar fi: extracția în câmp electric pulsatoriu, extracția asistată de enzime, extracția cu lichide sub presiune, extracția cu fluide supercritice. Materialul biologic supus extracției poate fi prelucrat în același timp și pentru valorificarea altor componente valoroase: polifenoli, antociani, proteine, etc..The process according to the invention has many advantages: the mass of biological material processed per batch is at least 100 times higher than in the batch process, the phenomenon of foaming of the biological material is avoided and thus unwanted events, the extraction efficiency of natural substances increases by up to minimum 25%, significantly reduces the extraction time, obtains a product of high purity and superior quality in terms of chemical composition compared to other methods and systems of extraction in the microwave field and / or unconventional methods, such as be: pulsed electric field extraction, enzyme-assisted extraction, extraction with pressurized liquids, extraction with supercritical fluids. The biological material subjected to extraction can be processed at the same time for the recovery of other valuable components: polyphenols, anthocyanins, proteins, etc ..
Problema tehnică pe care o rezolvă invenția constă în proiectarea unui nou tip de reactor continuu pentru obținerea substanțelor naturale din material biologic crud sau uscat pentru extracțiile asistate de microunde și ultrasunete și metoda de obținere a acestor substanțe naturale cu noul tip de reactor.The technical problem solved by the invention consists in the design of a new type of continuous reactor for obtaining natural substances from raw or dry biological material for microwave and ultrasonic assisted extractions and the method of obtaining these natural substances with the new type of reactor.
Reactorul chimic utilizat pentru extracția asistată de microunde și ultrasunete (MW/LIS), conform invenției, constă în aceea că materialul biologic, alcătuit din plante măcinate sau lemn măcinat sau semințe măcinate sau rășini măcinate amestecate cu solvent (polar sau nepolar) sunt introduse cu ajutorul unei pompe de proces în reactorul continuu în zona de extracție. Amestecul material biologic/solvent este supus iradierii simultane ultrasunete - microunde, la puteri de ultrasunete cuprinse între 100 - 500 W/l și puteri de microunde de 200 - 1000 W/l și o frecvență de 2450 MHz, la temperatura de 40 - 110°C, presiune normală, timp de 10 - 120 min., la un debit al pompei de 1 - 2 l/min..The chemical reactor used for assisted microwave and ultrasonic extraction (MW / LIS) according to the invention consists in that the biological material, consisting of ground plants or ground wood or ground seeds or ground resins mixed with solvent (polar or non-polar) are introduced with using a process pump in the continuous reactor in the extraction area. The biological material / solvent mixture is subjected to simultaneous ultrasonic-microwave irradiation, at ultrasonic powers between 100 - 500 W / l and microwave powers of 200 - 1000 W / l and a frequency of 2450 MHz, at a temperature of 40 - 110 ° C, normal pressure, for 10 - 120 min., At a pump flow of 1 - 2 l / min.
Procedeul conform invenției prezintă numeroase avantaje :The process according to the invention has many advantages:
• Obținerea de uleiuri volatile pure ;• Obtaining pure volatile oils;
• Obținerea de polifenoli, antociani și proteine ;• Obtaining polyphenols, anthocyanins and proteins;
• Timp de extracție scăzut;• Low extraction time;
• Temperatura de extracție controlată în funcție de produsul de extracție care dorește să se obțină ;• Extraction temperature controlled according to the extraction product you want to obtain;
• Temperatură scăzută de extracție pentru evitarea degradării termice a compușilor termolabili;• Low extraction temperature to avoid thermal degradation of thermolabile compounds;
• Volum mare de extracție ;• High extraction volume;
¢-2015-- 000351 9 -ci- 2015 • Randament de extracție ridicat;¢ -2015-- 000351 9 -ci- 2015 • High extraction efficiency;
• Extracția asistată de microunde și ultrasunete este un procedeu rapid, selectiv, nepoluant, care decurge cu viteză mare de extracție, ușor de controlat din punct de vedere tehnologic.• Microwave and ultrasonic assisted extraction is a fast, selective, non-polluting process, which proceeds with high extraction speed, easy to control from a technological point of view.
într-un vas de stocare se prepară amestecul material biologic/solvent.și se omogenizează, astfel încât toată cantitatea de plantă, lemn sau sămânță să fie în contact cu solventul. în reactorul continuu se introduce amestecul material biologic/solvent cu ajutorul pompei și se pornesc sursele de ultrasunete și microunde. Se reglează parametrii operaționali: timp, temperatură, putere de ultrasunete, putere de microunde, debitul pompei. Extracția compușilor biologic activi se realizează în condițiile tehnologice impuse. în funcție de natura produsului biologic activ obținut, și anume : ulei esențial, amestec de polifenoli, antociani sau proteine, aceștia se răcesc la temperatura camerei, se condiționează prin filtrare, uscare, centrifugare sau liofilizate și se depozitează.In a storage vessel the biological material / solvent mixture is prepared and homogenized so that the entire amount of plant, wood or seed is in contact with the solvent. The biological material / solvent mixture is introduced into the continuous reactor by means of the pump and the ultrasound and microwave sources are switched on. The operating parameters are adjusted: time, temperature, ultrasonic power, microwave power, pump flow. The extraction of biologically active compounds is performed under the imposed technological conditions. Depending on the nature of the biologically active product obtained, namely: essential oil, mixture of polyphenols, anthocyanins or proteins, they are cooled to room temperature, conditioned by filtration, drying, centrifugation or lyophilized and stored.
Se prezintă, în continuare, câteva exemple nelimitative de aplicare a prezentei invenții.The following are some non-limiting examples of application of the present invention.
Exemplul 1. Se cântăresc pe balanța tehnică 5 Kg rozmarin (Rosmarinus Officinalis) uscat (proveniență UE), măcinat la o granulație de aproximativ 0.5 mm, se introduc în vasul de stocare peste care se adaugă 20 L apă deionizată, raport masic planta/solvent = 1 :4. Amestecul se omogenizează cu un omogenizator mecanic timp de 30 min. la temperatura camerei, la o turație de 50 rpm. Se introduc furtunele de absorbție și evacuare ale pompei în vasul de stocare, se cuplează pompa la reactorul continuu, și se pornește la un debit de 1 L/min.. Se pornesc sursele de ultrasunete la o putere de 200 W/L și de microunde la o putere de 400 W/L, se adaptează sistemul Clevenger de colectare al uleiului volatil și se reglează timpul de extracție la 90 min. După 90 min. extracția uleiului volatil a fost completă. Uleiul volatil, se separă de apă și se usucă pe Na2SO4 anhidru. Astfel obținut uleiul volatil se depozitează în vase închise la culoare în spații ferite de lumină și căldură.Example 1. Weigh on the technical balance 5 Kg dried rosemary (Rosmarinus Officinalis) (EU origin), ground to a granulation of approximately 0.5 mm, place in the storage vessel over which 20 L deionized water is added, mass ratio plant / solvent = 1: 4. The mixture is homogenized with a mechanical homogenizer for 30 min. at room temperature at 50 rpm. Insert the pump suction and discharge hoses into the storage vessel, connect the pump to the continuous reactor, and start at a flow rate of 1 L / min. Turn on the ultrasound sources at a power of 200 W / L and microwave at a power of 400 W / L, the Clevenger volatile oil collection system is adapted and the extraction time is set to 90 min. After 90 min. volatile oil extraction was complete. The volatile oil is separated from the water and dried over anhydrous Na 2 SO 4 . Thus obtained the volatile oil is stored in dark vessels in places away from light and heat.
Exemplul 2. Se cântăresc pe balanța tehnică 10 Kg fructe de coacăz negru ( Ribes nigrum) proaspăt și se amestecă cu 10 L apă deionizată și 10 L alcool etilic 97 grade de proveniență vegetală în vasul de stocare. Amestecul se omogenizează cu un omogenizator mecanic timp de 30 min. la temperatura camerei, la o turație de 100 rpm. Se introduc furtunul de absorbție al pompei în vasul de stocare iar cel de evacuare în vasul de colectare, se cuplează pompa la reactorul continuu, și se pornește la un debit de 0.5 L/min.. Se pornesc sursele de ultrasunete la o putere de 100 W/L și de microunde la o putere de 300 W/L, se 4Example 2. Weigh 10 Kg of fresh currant (Ribes nigrum) fruit on the technical balance and mix with 10 L of deionized water and 10 L of ethyl alcohol 97 degrees of vegetable origin in the storage vessel. The mixture is homogenized with a mechanical homogenizer for 30 min. at room temperature at 100 rpm. Insert the pump suction hose into the storage vessel and the discharge hose into the collection vessel, connect the pump to the continuous reactor, and start at a flow rate of 0.5 L / min. Turn on the ultrasound sources at a power of 100 W / L and microwave at a power of 300 W / L, 4
-2015-- 000351 9 -01* 2015 reglează timpul de extracție la 120 min. După 120 min. se colectează amestecul de polifenoli obținut , care se separă prin filtrare. Amestecul de polifenoli se concentrează prin liofilizare. Astfel obținut acesta se depozitează în vase închise la culoare în spații ferite de lumină și căldură.-2015-- 000351 9 -01 * 2015 sets the extraction time to 120 min. After 120 min. collect the obtained polyphenol mixture, which is separated by filtration. The mixture of polyphenols is concentrated by lyophilization. Thus obtained, it is stored in dark vessels in places away from light and heat.
Exemplul 3. Se cântăresc pe balanța tehnică 3 Kg miez de nucă măcinat la o granulație de 0.6 mm (Juglans regia L.) și se amestecă cu 6 L hexan în vasul de stocare. Amestecul se omogenizează cu un omogenizator mecanic timp de 40 min. la temperatura camerei, la o turație de 30 rpm. Se introduc furtunul de absorbție al pompei în vasul de stocare iar cel de evacuare în vasul de colectare, se cuplează pompa la reactorul continuu, și se pornește la un debit de 0.2 L/min.. Se pornesc sursele de ultrasunete la o putere de 300 W/L și de microunde la o putere de 600 W/L, se reglează timpul de extracție la 60 min. După 60 min. se colectează amestecul obținut , care se separă prin filtrare. Amestecul de solvent/ulei gras obținut se distilă în vid pentru eliminarea solventului, se spală cu apă distilată de 3 ori și se usucă pe Na2SO4 anhidru. Astfel obținut uleiul gras se depozitează în vase închise la culoare în spații ferite de lumină și căldură.Example 3. Weigh on the technical balance 3 Kg of ground walnut kernels to a granulation of 0.6 mm (Juglans regia L.) and mix with 6 L of hexane in the storage vessel. The mixture is homogenized with a mechanical homogenizer for 40 min. at room temperature at 30 rpm. Insert the pump suction hose into the storage vessel and the discharge hose into the collection vessel, connect the pump to the continuous reactor, and start at a flow rate of 0.2 L / min. Start the ultrasound sources at a power of 300 W / L and microwave at a power of 600 W / L, set the extraction time to 60 min. After 60 min. collect the obtained mixture, which is separated by filtration. The solvent / fatty oil mixture obtained was distilled in vacuo to remove the solvent, washed with distilled water 3 times and dried over anhydrous Na 2 SO 4 . Thus obtained the fatty oil is stored in dark vessels in places away from light and heat.
Claims (4)
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ROA201500035A RO130896A0 (en) | 2015-01-19 | 2015-01-19 | Continuous flow reactor for microwave- and ultrasound-assisted extraction of biologically active compounds from plants |
| EP16740464.9A EP3283605A4 (en) | 2015-01-19 | 2016-01-18 | Process and installation for extraction of biological active compounds from plants and continuous reactor for ultrasound and microwave assisted extraction of biological active compounds from plants |
| PCT/RO2016/050001 WO2016118034A2 (en) | 2015-01-19 | 2016-01-18 | Process and installation for extraction of biological active compounds from plants and continuous reactor for ultrasound and microwave assisted extraction of biological active compounds from plants |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ROA201500035A RO130896A0 (en) | 2015-01-19 | 2015-01-19 | Continuous flow reactor for microwave- and ultrasound-assisted extraction of biologically active compounds from plants |
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| Publication Number | Publication Date |
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| RO130896A0 true RO130896A0 (en) | 2016-02-26 |
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| ROA201500035A RO130896A0 (en) | 2015-01-19 | 2015-01-19 | Continuous flow reactor for microwave- and ultrasound-assisted extraction of biologically active compounds from plants |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP3283605A4 (en) |
| RO (1) | RO130896A0 (en) |
| WO (1) | WO2016118034A2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| BR102017021157B1 (en) * | 2017-10-02 | 2022-07-26 | Baldo S/A Comércio Indústria E Exportação | PROCESS FOR OBTAINING ROASTED MATE EXTRACT |
| CN107930182B (en) * | 2017-12-29 | 2024-05-24 | 山西鑫旭生物科技有限公司 | Plant active substance extraction element |
| IT201900020630A1 (en) * | 2019-11-08 | 2021-05-08 | Univ Degli Studi Genova | Process and system for the extraction of molecules from solid particle matrices |
| KR102311749B1 (en) * | 2019-12-31 | 2021-10-13 | 한국과학기술연구원 | Method of continuously producing cannabinol from Cannabis sp. and uses thereof |
| CN111704961B (en) * | 2020-06-29 | 2022-04-08 | 山东省林业保护和发展服务中心 | Walnut male flower essential oil and extraction method thereof |
| CN113563974A (en) * | 2021-08-19 | 2021-10-29 | 广州市藻德道科技有限公司 | Method for ultrasonically extracting ginger essential oil without organic solvent |
| FR3134014B1 (en) | 2022-04-01 | 2024-03-29 | Innovation & Dev Company | microwave extraction oven for the continuous heat treatment of organic products in solid or pasty state |
| CN115671787A (en) * | 2022-11-21 | 2023-02-03 | 华南理工大学 | Method for accurately controlling and extracting purple-flower kaempferia galanga bioactive substances in grading manner by using high-voltage pulse electric field |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1336968C (en) * | 1989-05-16 | 1995-09-12 | J. R. Jocelyn Pare | Microwave-assisted natural products extraction |
| FR2705035B1 (en) * | 1993-05-11 | 1995-08-04 | Archimex Pibs | Process and installation for solvent-free extraction of natural products by microwave. |
| RU2316375C2 (en) * | 2005-08-02 | 2008-02-10 | Общество с ограниченной ответственностью "Славянский чай" | Method for producing of dry water-soluble extract from raw plant material |
| CN102179062A (en) * | 2010-03-02 | 2011-09-14 | 上海远跃轻工机械有限公司 | Ultrasound/microwave continuous countercurrent extraction device and method |
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2015
- 2015-01-19 RO ROA201500035A patent/RO130896A0/en unknown
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2016
- 2016-01-18 WO PCT/RO2016/050001 patent/WO2016118034A2/en active Application Filing
- 2016-01-18 EP EP16740464.9A patent/EP3283605A4/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| WO2016118034A2 (en) | 2016-07-28 |
| EP3283605A4 (en) | 2018-11-14 |
| EP3283605A2 (en) | 2018-02-21 |
| WO2016118034A3 (en) | 2016-10-06 |
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