TWI680012B - High-efficiency ultrasonic extraction equipment and method for improving supercritical extraction efficiency - Google Patents

High-efficiency ultrasonic extraction equipment and method for improving supercritical extraction efficiency Download PDF

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TWI680012B
TWI680012B TW107137111A TW107137111A TWI680012B TW I680012 B TWI680012 B TW I680012B TW 107137111 A TW107137111 A TW 107137111A TW 107137111 A TW107137111 A TW 107137111A TW I680012 B TWI680012 B TW I680012B
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tank
pressure reaction
extraction
reaction tank
liquid raw
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TW202015802A (en
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陳嘉勳
康順安
陳勝益
黃冠琳
陳怡璇
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聯盛科技有限公司
鞏骨力生物科技股份有限公司
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Priority to CN201910532607.7A priority patent/CN111068358A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0203Solvent extraction of solids with a supercritical fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0261Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
    • B01D11/0265Applying ultrasound
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0403Solvent extraction of solutions which are liquid with a supercritical fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0419Solvent extraction of solutions which are liquid in combination with an electric or magnetic field or with vibrations
    • B01D11/0423Applying ultrasound
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/002Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • B01J3/042Pressure vessels, e.g. autoclaves in the form of a tube

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

本發明係提供一種高效率超音波萃取設備與提升超臨界萃取效率之方法,該高效率超音波萃取設備係包含有至少一高壓反應槽與一超臨界流體容器、一液體原料罐、若干高壓幫浦與控制閥,該高壓反應槽之蓋體內更設置有朝內延伸之一超音波棒,用以可於超臨界流體混合液體原料進行萃取之過程中,同時對液體原料進行超音波振盪,以萃取、分離出對人體有益之營養成分,進而可提高該高壓反應槽之萃取效率、縮短萃取時間。 The invention provides a high-efficiency ultrasonic extraction equipment and a method for improving the supercritical extraction efficiency. The high-efficiency ultrasonic extraction equipment includes at least a high-pressure reaction tank and a supercritical fluid container, a liquid raw material tank, and a plurality of high-pressure helpers. For Puhe control valve, a cover of the high pressure reaction tank is further provided with an inwardly extending ultrasonic rod, which can be used for supercritical fluid mixing of liquid raw materials during the extraction process. Extracting and separating nutritional components that are beneficial to the human body, thereby improving the extraction efficiency and shortening the extraction time of the high-pressure reaction tank.

Description

高效率超音波萃取設備與提升超臨界萃取效率之方法 High-efficiency ultrasonic extraction equipment and method for improving supercritical extraction efficiency

本發明係與超臨界萃取設備有關,更詳而言之是指一種高效率超音波萃取設備與提升超臨界萃取效率之方法者。 The invention relates to supercritical extraction equipment, and more specifically refers to a high-efficiency ultrasonic extraction equipment and a method for improving supercritical extraction efficiency.

按,習知超臨界萃取、分離天然物營養成分之製程,主要係利用超臨界狀態之二氧化碳流體於高壓、低溫條件下自天然物萃取出營養成分。而為了提升習知超臨界製程之萃取效率,有業者在進行萃取步驟前,先將液體原料(待萃取物粉碎後浸泡於酒精)進行超音波振盪,如中華民國發明第I604848號「蜂膠萃取物的萃取方法」專利所示,其係蜂膠原塊破碎浸泡酒精後以超音波振盪法進行溶解獲得一粗萃物,再將該粗萃物注入高壓超臨界萃取槽中進行萃取步驟,萃取步驟之條件為壓力範圍介於3600psi至4000psi之間,溫度範圍係介於46℃至50℃之間萃取80分鐘至120分鐘,藉以可獲得阿特比靈(artepillin C)成分,萃取效率相較於傳統超臨界製程有相當的提升。 According to the knowledge, the process of supercritical extraction and separation of natural nutrients is mainly used to extract nutrition from natural substances under high pressure and low temperature conditions by using supercritical carbon dioxide fluid. In order to improve the extraction efficiency of the conventional supercritical process, some practitioners first perform ultrasonic vibration on the liquid raw materials (after crushing the extract and soak it in alcohol) before performing the extraction step, such as the invention of the Republic of China No. I604848 "Extraction of Propolis Extract As shown in the "Method" patent, the collagen collagen is crushed and soaked in alcohol, and then dissolved by ultrasonic vibration to obtain a crude extract. The crude extract is then injected into a high-pressure supercritical extraction tank for the extraction step. The conditions of the extraction step are: The pressure range is between 3600 psi and 4000 psi, and the temperature range is between 46 ° C and 50 ° C. Extraction is 80 minutes to 120 minutes, so that Artepillin C can be obtained. The extraction efficiency is compared with traditional supercritical. The process has improved considerably.

換言之,前述專利藉由在傳統超臨界萃取步驟前先進行超音波振盪,可明顯地提升萃取之效率。不過,前 述專利之萃取時間仍需80分鐘至120分鐘,萃取效率仍有提升之空間,惟,目前為止,除了前述專利之技術外,目前並無更佳之技術。 In other words, the aforementioned patent can significantly improve the extraction efficiency by performing ultrasonic oscillation before the traditional supercritical extraction step. However, before The extraction time of said patent still needs 80 minutes to 120 minutes, and there is still room for improvement in extraction efficiency, but so far, except for the aforementioned patent technology, there is currently no better technology.

本發明之主要目的即在提供一種高效率超音波萃取設備與提升超臨界萃取效率之方法,其係於萃取步驟中同時進行超音波振盪,且產生超音波振盪之超音波棒係直接伸入作用於液體原料,可確實有效地提升萃取效率及縮短萃取時間,結構簡單,甚具經濟價值者。 The main object of the present invention is to provide a high-efficiency ultrasonic extraction device and a method for improving the supercritical extraction efficiency. The ultrasonic rods are simultaneously oscillated in the extraction step, and the ultrasonic rods that generate ultrasonic oscillations are directly extended. For liquid raw materials, it can effectively improve the extraction efficiency and shorten the extraction time. It has a simple structure and is of great economic value.

緣是,為達成前述之目的,本發明係提供一種高效率超音波萃取設備,包含有至少一高壓反應槽,用以可自天然物萃取、分離出對人體有益之營養成分,包含開口朝上之一槽體,該槽體底端設有一出料口,供輸出萃取液,一蓋體,蓋設於該槽體之頂端開口,一電加熱器,設置於該槽體,用以加熱進入該槽體內之液體原料,一超音波棒,設置於該蓋體內而伸入槽體;一超臨界流體容器與一液體原料罐,連接該高壓反應槽,用以分別提供超臨界流體與液體原料,該超臨界流體係超臨界狀態二氧化碳流體;若干高壓幫浦,設置於該超臨界流體容器、液體原料罐與高壓反應槽之間,用以將超臨界流體與液體原料加壓輸送至高壓反應槽;複數控制閥,分別設置於各該超臨界流體容器、液體原料罐與高壓反應槽之間,用以可分別控制超臨界流體、液體原料 及萃取液之流向。 The reason is that, in order to achieve the foregoing object, the present invention provides a high-efficiency ultrasonic extraction device, which includes at least one high-pressure reaction tank for extracting and separating nutrient components that are beneficial to the human body from natural objects, including openings facing upward. A tank body, the bottom end of the tank body is provided with a discharge port for outputting the extraction liquid, a cover body is disposed on the top opening of the tank body, and an electric heater is provided in the tank body for heating and entering The liquid raw material in the tank, an ultrasonic rod, is arranged in the cover body to extend into the tank body; a supercritical fluid container and a liquid raw material tank are connected to the high pressure reaction tank to provide supercritical fluid and liquid raw materials respectively The supercritical flow system is in a supercritical state carbon dioxide fluid; several high-pressure pumps are arranged between the supercritical fluid container, the liquid raw material tank and the high-pressure reaction tank, and are used to pressurize the supercritical fluid and the liquid raw material to the high-pressure reaction. A plurality of control valves are respectively provided between the supercritical fluid container, the liquid raw material tank and the high-pressure reaction tank, so as to control the supercritical fluid and liquid raw materials separately. And the direction of the extract.

較佳地,係包含有一第一高壓反應槽與若干第二高壓反應槽,該超臨界流體容器與液體原料罐係連接第一高壓反應槽之槽體頂端與底端,該第一高壓反應槽之槽體頂端、底端並透過二連接管合併後連接第二高壓反應槽之槽體頂端,用以可供該第一高壓反應槽內之萃取液再輸送至第二高壓反應槽進行萃取。 Preferably, the system comprises a first high-pressure reaction tank and a plurality of second high-pressure reaction tanks. The supercritical fluid container and the liquid raw material tank are connected to the top and bottom ends of the tank body of the first high-pressure reaction tank. The first high-pressure reaction tank The top and bottom ends of the tank body are combined through two connecting pipes and connected to the top end of the tank body of the second high pressure reaction tank, so that the extraction liquid in the first high pressure reaction tank can be transported to the second high pressure reaction tank for extraction.

較佳地,該二連接管上並分別設有該控制閥。 Preferably, the two connecting pipes are respectively provided with the control valves.

較佳地,該超臨界流體容器與液體原料罐之輸出管路係合併後再連接第一高壓反應槽之槽體頂端、底端,各該輸出管路上分別設有該高壓幫浦。 Preferably, the output pipelines of the supercritical fluid container and the liquid raw material tank are combined and then connected to the top and bottom ends of the tank body of the first high-pressure reaction tank, and each of the output pipelines is provided with the high-pressure pump.

較佳地,該超臨界流體容器與液體原料罐之輸出管路上更分別設有該控制閥,係介於各該高壓幫浦與第一高壓反應槽之槽體頂端、底端之間。 Preferably, the control pipe is further provided on the output pipeline of the supercritical fluid container and the liquid raw material tank, which is interposed between each of the high-pressure pump and the top and bottom ends of the tank body of the first high-pressure reaction tank.

較佳地,該出料口上設有一控制閥。 Preferably, a control valve is provided on the discharge port.

較佳地,各該控制閥包含複數高壓閥、單向閥與若干背壓閥,各該高壓閥係分別設置於超臨界流體容器與液體原料罐之輸出管路、二連接管及各高壓反應槽之出料口,用以供控制超臨界流體容器與液體原料罐之輸出壓力、啟閉及各高壓反應槽是否輸出萃取液,各該單向閥係分別設置於超臨界流體容器與液體原料罐之輸出管路及連接該第一高壓反應槽之槽體底端之連接管,用以防止加壓之超臨界 流體與液體原料回流及防止該連接管內之萃取液朝第一高壓反應槽之槽體底端回流,該背壓閥係設置於連接該第一、第二高壓反應槽之槽體頂端之連接管,用以可控制該連接管所需壓力與流量。 Preferably, each of the control valves includes a plurality of high-pressure valves, a one-way valve and a plurality of back pressure valves, and each of the high-pressure valves is respectively provided in an output pipeline, two connecting pipes and high-pressure reactions of a supercritical fluid container and a liquid raw material tank. The outlet of the tank is used to control the output pressure, opening and closing of the supercritical fluid container and the liquid raw material tank, and whether each high-pressure reaction tank outputs the extraction liquid. Each of the one-way valve systems is respectively provided in the supercritical fluid container and the liquid raw material. The output pipe of the tank and the connecting pipe connected to the bottom end of the tank body of the first high-pressure reaction tank are used to prevent supercritical pressure The backflow of fluid and liquid raw materials and preventing the extraction liquid in the connecting tube from flowing back toward the bottom end of the tank of the first high-pressure reaction tank. The back pressure valve is provided at the top of the tank body connecting the first and second high-pressure reaction tanks. Pipe for controlling the pressure and flow required by the connecting pipe.

此外,本發明更提供一種提升超臨界萃取效率之方法,主要係於超臨界流體混合液體原料進行萃取之過程中,同時對液體原料進行超音波振盪,以萃取、分離出對人體有益之營養成分,進而可提高該高壓反應槽之萃取效率、縮短萃取時間。 In addition, the present invention further provides a method for improving supercritical extraction efficiency, which is mainly in the process of supercritical fluid mixed liquid raw material extraction, and at the same time ultrasonically oscillates the liquid raw material to extract and separate nutritious components that are beneficial to the human body. Therefore, the extraction efficiency and the extraction time of the high-pressure reaction tank can be improved.

較佳地,係於至少一高壓反應槽內進行萃取過程,該高壓反應槽一端連接有一超臨界流體容器與一液體原料罐,供將超臨界流體與液體原料混合後輸入高壓反應槽,該高壓反應槽包含開口朝上之一槽體,該槽體底端設有一出料口,供輸出萃取液,一蓋體,蓋設於該槽體之頂端開口,一超音波棒,設置於該蓋體內而伸入槽體。 Preferably, the extraction process is performed in at least one high-pressure reaction tank. One end of the high-pressure reaction tank is connected with a supercritical fluid container and a liquid raw material tank for mixing the supercritical fluid and the liquid raw material into the high-pressure reaction tank. The reaction tank includes a tank body with an opening facing upwards. A discharge port is provided at the bottom end of the tank body for outputting extraction liquid, a cover body is disposed on the top opening of the tank body, and an ultrasonic rod is disposed on the cover. The body extends into the trough.

較佳地,係包含有一第一高壓反應槽與若干第二高壓反應槽,該超臨界流體容器與液體原料罐係連接第一高壓反應槽之槽體頂端與底端,該第一高壓反應槽之槽體頂端、底端並透過二連接管合併後連接第二高壓反應槽之槽體頂端,用以可供該第一高壓反應槽內之萃取液再輸送至第二高壓反應槽進行萃取、分離。 Preferably, the system comprises a first high-pressure reaction tank and a plurality of second high-pressure reaction tanks. The supercritical fluid container and the liquid raw material tank are connected to the top and bottom ends of the tank body of the first high-pressure reaction tank. The first high-pressure reaction tank The top and bottom ends of the tank body are combined through two connecting pipes and connected to the top end of the tank body of the second high-pressure reaction tank, so that the extraction liquid in the first high-pressure reaction tank can be transported to the second high-pressure reaction tank for extraction, Separation.

10‧‧‧高效率超音波萃取設備 10‧‧‧High-efficiency ultrasonic extraction equipment

12‧‧‧高壓反應槽 12‧‧‧ high pressure reaction tank

13‧‧‧超臨界流體容器 13‧‧‧Supercritical fluid container

14‧‧‧液體原料罐 14‧‧‧Liquid raw material tank

15、16‧‧‧高壓幫浦 15, 16‧‧‧ high pressure pump

22‧‧‧槽體 22‧‧‧ trough

221‧‧‧出料口 221‧‧‧Discharge port

24‧‧‧蓋體 24‧‧‧ Cover

26‧‧‧電加熱器 26‧‧‧ Electric heater

28‧‧‧超音波棒 28‧‧‧ Ultrasonic Stick

32、42‧‧‧輸出管路 32, 42‧‧‧ output lines

72‧‧‧高壓閥 72‧‧‧ high pressure valve

74‧‧‧單向閥 74‧‧‧Check valve

80‧‧‧高效率超音波萃取設備 80‧‧‧High-efficiency ultrasonic extraction equipment

82‧‧‧高壓反應槽 82‧‧‧High-pressure reaction tank

84、86‧‧‧連接管 84, 86‧‧‧ connecting pipe

88‧‧‧背壓閥 88‧‧‧Back pressure valve

第一圖係本發明一較佳實施例之系統圖。 The first diagram is a system diagram of a preferred embodiment of the present invention.

第二圖係本發明另一較佳實施例之系統圖。 The second diagram is a system diagram of another preferred embodiment of the present invention.

以下,茲舉本發明數個較佳實施例,並配合圖式做進一步之詳細說明如後:首先,請參閱第一圖所示,本發明一較佳實施例之高效率超音波萃取設備10,係包含有一高壓反應槽12、一超臨界流體容器13、一液體原料罐14、二高壓幫浦15、16與複數控制閥。 In the following, several preferred embodiments of the present invention are given, and further detailed description is given in conjunction with the drawings as follows: First, please refer to the first figure, a high-efficiency ultrasonic extraction device 10 according to a preferred embodiment of the present invention. It consists of a high-pressure reaction tank 12, a supercritical fluid container 13, a liquid raw material tank 14, two high-pressure pumps 15, 16 and a plurality of control valves.

該高壓反應槽12,具有一槽體22、一蓋體24及一電加熱器26等習知超臨界萃取槽之構件,該槽體22底端係設有一出料口221,供輸出萃取液,該電加熱器26係用以加熱進入槽體22內之液體原料,本發明更於該蓋體24內設有一超音波棒28,該超音波棒28係伸入槽體22約1/2至1/3深度,而可對該液體原料罐14輸入槽體22之液體原料進行24KHz至40KHz間頻率之振盪,本實施例採40KHz高頻的振盪,藉以可萃取、分離出對人體有益之營養成分。 The high-pressure reaction tank 12 includes components of a conventional supercritical extraction tank, such as a tank body 22, a cover body 24, and an electric heater 26. The bottom end of the tank body 22 is provided with a discharge port 221 for outputting the extraction liquid. The electric heater 26 is used to heat the liquid raw material entering the tank 22. The present invention further provides an ultrasonic rod 28 in the cover 24. The ultrasonic rod 28 extends into the tank 22 about 1/2 to 1 / 3 depth, and the liquid raw material in the liquid raw material tank 14 input tank 22 can be oscillated at a frequency between 24KHz and 40KHz. In this embodiment, a high-frequency oscillation at 40KHz is used to extract and separate nutritional components that are beneficial to the human body. .

該超臨界流體容器13與液體原料罐14,分別為CO2鋼瓶、用以儲存並提供超臨界CO2流體,及容納並提供液體原料,二者之輸出管路32、42係合併後再分開連接高壓反應槽12之槽體22頂端、底端。 The supercritical fluid container 13 and the liquid raw material tank 14 are respectively a CO2 steel cylinder for storing and supplying a supercritical CO 2 fluid, and containing and supplying a liquid raw material. The output pipes 32 and 42 of the two are combined and then connected separately. The top and bottom ends of the tank body 22 of the high-pressure reaction tank 12.

該二高壓幫浦15、16,分別設置於該超臨界流體容器13與液體原料罐14之輸出管路32、42,用以可將該超臨界流體與液體原料加壓、計量輸送至高壓反應槽12。 The two high-pressure pumps 15 and 16 are respectively arranged in the output lines 32 and 42 of the supercritical fluid container 13 and the liquid raw material tank 14 so as to pressurize and meter the supercritical fluid and the liquid raw material to a high-pressure reaction. Slot 12.

各該控制閥,包含五高壓閥72與二單向閥74,各該高壓閥72係分別設置於二輸出管路32、42合併前、後位置及高壓反應槽12之出料口221,用以可供控制該超臨界流體容器13與液體原料罐14之輸出壓力、啟閉及控制高壓反應槽12是否輸出萃取液。該二單向閥74係分別設置於二輸出管路32、42合併前之位置,用以防止加壓之超臨界流體與液體原料回流。 Each of the control valves includes five high-pressure valves 72 and two one-way valves 74. Each of the high-pressure valves 72 is respectively provided at the two output lines 32 and 42 and merges the front and rear positions and the discharge port 221 of the high-pressure reaction tank 12. It can be used for controlling the output pressure of the supercritical fluid container 13 and the liquid raw material tank 14, opening and closing, and controlling whether the high-pressure reaction tank 12 outputs the extraction liquid. The two non-return valves 74 are respectively disposed at the positions before the two output lines 32 and 42 are combined to prevent the backflow of the pressurized supercritical fluid and liquid raw materials.

藉此,本發明該高效率超音波萃取設備10之操作方式,係先打開該超臨界流體容器13與液體原料罐14,利用該二高壓幫浦15、16控制超臨界流體容器13與液體原料罐14之輸出壓力與劑量,再利用各該高壓閥72控制高壓反應槽12之壓力,並透過該電加熱器26控制高壓反應槽12之溫度,操作條件例如:壓力2000-4000psi、溫度40-60℃、超臨界二氧化碳流體流速6-9L/hr,詳細之萃取、分離步驟與習知超臨界流體萃取設備類似,此處不予贅述,本發明該高效率超音波萃取設備10之特色、功效係在於:該高壓反應槽12內設有直接伸入液體原料內之超音波棒28,該超音波棒28所產生之高頻振盪,可直接作用於液體原料,俾可大大地提升萃取效率(對人體有益營養成 分之含量)及縮短萃取時間。 Therefore, the operation mode of the high-efficiency ultrasonic extraction device 10 of the present invention is to first open the supercritical fluid container 13 and the liquid raw material tank 14 and use the two high-pressure pumps 15 and 16 to control the supercritical fluid container 13 and the liquid raw material. The output pressure and dose of the tank 14 are then controlled by the high-pressure valve 72 to control the pressure of the high-pressure reaction tank 12 and the temperature of the high-pressure reaction tank 12 is controlled by the electric heater 26. Operating conditions such as: pressure 2000-4000psi, temperature 40- 60 ° C, supercritical carbon dioxide fluid flow rate 6-9L / hr, detailed extraction and separation steps are similar to conventional supercritical fluid extraction equipment, which will not be repeated here. The features and effects of the high-efficiency ultrasonic extraction equipment 10 of the present invention are: : The high-pressure reaction tank 12 is provided with an ultrasonic rod 28 directly protruding into the liquid raw material. The high-frequency oscillation generated by the ultrasonic rod 28 can directly act on the liquid raw material, which can greatly improve the extraction efficiency (for the human body). Beneficial nutrition Content) and shorten the extraction time.

例如,如表一與表二所示,透過本發明對蜂膠及靈芝進行萃取,與習知無超音波之超臨界萃取製程之比較,經實驗証明,本發明對同一種天然物可有效縮短萃取時間約1/3左右,且營養成分之萃取量更高,如下: For example, as shown in Tables 1 and 2, when the present invention is used to extract propolis and ganoderma, compared with the conventional supercritical extraction process without ultrasonic waves, experiments have proved that the present invention can effectively shorten the extraction of the same natural substance. The time is about 1/3, and the extraction amount of nutrients is higher, as follows:

前揭對蜂膠及靈芝進行萃取時,操作條件為溫度48℃,壓力3800psi。 When the propolis and ganoderma are extracted before peeling, the operating conditions are 48 ° C and 3800psi.

由上可知,本發明該高效率超音波萃取設備藉由在高壓反應槽內設置可直接伸入液體原料之超音波棒之結構,可使該超音波棒所產生之高頻振盪直接作用於液體原料,進而可有效地提升萃取效率(營養成分之萃取量更高) 及縮短萃取時間,雖然結構簡單,但甚具經濟價值。 It can be known from the above that the high-efficiency ultrasonic extraction device of the present invention has a structure in which a high-frequency ultrasonic rod capable of directly penetrating liquid raw materials is arranged in a high-pressure reaction tank, so that the high-frequency oscillation generated by the ultrasonic rod can directly act on the liquid. Raw materials, which can effectively improve the extraction efficiency (higher extraction of nutrients) And shorten the extraction time, although the structure is simple, but it is very economical.

其次,該二輸出管路32、42合併後之二高壓閥72,係可供決定超臨界流體與液體原料係分別或同時流入高壓反應槽12之槽體22頂端或底端,主要係視萃取原料之特性、萃取效果而調整。 Secondly, the combined high pressure valve 72 of the two output lines 32 and 42 can be used to determine whether the supercritical fluid and the liquid raw material flow into the top or bottom of the tank 22 of the high pressure reaction tank 12 separately or at the same time, mainly depending on the extraction Adjust the characteristics of raw materials and extraction effect.

此外,本發明可再增設若干高壓反應槽,如第二圖所示,係本發明另一較佳實施例之高效率超音波萃取設備80,其構成大體上與該高效率超音波萃取設備10相同,不同處在於:其除了前述該高壓反應槽12外(後稱第一高壓反應槽),更包含有另一相同構造之高壓反應槽82(後稱第二高壓反應槽),且,該第一高壓反應槽12之槽體22頂端、底端並透過二連接管84、86合併後連接第二高壓反應槽82之槽體頂端,用以可供該第一高壓反應槽12內之萃取液再輸送至第二高壓反應槽82進行萃取,此外,該連接管84上更設有一如前述之高壓閥72與一背壓閥88,該背壓閥88係可控制該連接管84所需壓力與流量,該連接管86上更設有如前述之一高壓閥72與一單向閥74。藉此,透過複數高壓反應槽12、82進行超臨界萃取,可減少萃取液中的成分種類、使萃取液之成分更為單純。 In addition, the present invention can further add a number of high-pressure reaction tanks, as shown in the second figure, which is a high-efficiency ultrasonic extraction device 80 according to another preferred embodiment of the present invention. The same, except that the high-pressure reaction tank 12 (hereinafter referred to as the first high-pressure reaction tank) further includes another high-pressure reaction tank 82 (hereinafter referred to as the second high-pressure reaction tank) having the same structure, and the The top and bottom ends of the tank 22 of the first high-pressure reaction tank 12 are combined through two connecting pipes 84 and 86 and connected to the top of the tank of the second high-pressure reaction tank 82 for extraction in the first high-pressure reaction tank 12. The liquid is sent to the second high-pressure reaction tank 82 for extraction. In addition, the connection pipe 84 is provided with a high-pressure valve 72 and a back pressure valve 88 as described above. The back pressure valve 88 can control the connection pipe 84. Pressure and flow, the connection pipe 86 is further provided with a high pressure valve 72 and a check valve 74 as described above. Thereby, supercritical extraction is performed through the plurality of high-pressure reaction tanks 12, 82, and the types of components in the extraction liquid can be reduced, and the components of the extraction liquid can be made simpler.

再者,由上可知,本發明更可提供一種提升超臨界萃取效率之方法,即於前述連接超臨界流體容器13與液體原料罐14之高壓反應槽12、72內設置一超音波棒28,該超音波棒28並伸入高壓反應槽12、72內,俾可於超臨界流體混合液體原料進行萃取之過程中,同時對液體原料進行 超音波振盪,以萃取、分離出對人體有益之營養成分,進而可提高該高壓反應槽之萃取效率、縮短萃取時間。 Furthermore, as can be seen from the above, the present invention can further provide a method for improving the supercritical extraction efficiency, that is, an ultrasonic rod 28 is provided in the high-pressure reaction tanks 12 and 72 connecting the supercritical fluid container 13 and the liquid raw material tank 14, The ultrasonic rod 28 extends into the high-pressure reaction tanks 12, 72, and can be used for the extraction of liquid raw materials in the process of mixing supercritical fluid with liquid raw materials. Ultrasonic vibration is used to extract and separate the nutritional components that are beneficial to the human body, thereby improving the extraction efficiency and shortening the extraction time of the high-pressure reaction tank.

惟,以上所述僅為本發明之數個較佳實施例,當不能以此限定本發明之申請專利保護範圍,舉凡依本發明之申請專利範圍及說明書內容所作之簡單的等效變化與替換,皆應仍屬於本發明申請專利範圍所涵蓋保護之範圍內。 However, the above are only a few preferred embodiments of the present invention. When the scope of patent protection of the present invention cannot be limited by this, for example, simple equivalent changes and replacements made according to the scope of patent application of the present invention and the contents of the description , All should still fall within the protection scope covered by the patent application scope of the present invention.

Claims (9)

一種高效率超音波萃取設備,包含有:至少一高壓反應槽,用以可自天然物萃取、分離出對人體有益之營養成分,包含開口朝上之一槽體,該槽體底端設有一出料口,供輸出萃取液,一蓋體,蓋設於該槽體之頂端開口,一電加熱器,設置於該槽體,用以加熱進入該槽體內之液體原料,一超音波棒,設置於該蓋體內而伸入槽體;一超臨界流體容器與一液體原料罐,連接該高壓反應槽,用以分別提供超臨界流體與液體原料,該超臨界流體係超臨界狀態二氧化碳流體;若干高壓幫浦,設置於該超臨界流體容器、液體原料罐與高壓反應槽之間,用以將超臨界流體與液體原料加壓輸送至高壓反應槽;及複數控制閥,分別設置於各該超臨界流體容器、液體原料罐與高壓反應槽之間,用以可分別控制超臨界流體、液體原料及萃取液之流向。A high-efficiency ultrasonic extraction device includes: at least one high-pressure reaction tank for extracting and separating nutritious ingredients that are beneficial to the human body from natural objects, and includes a tank with an opening facing upward, and a bottom end of the tank is provided with a The discharge port is for outputting the extraction liquid, a cover body is arranged on the top opening of the tank body, an electric heater is arranged on the tank body for heating the liquid raw materials entering the tank body, an ultrasonic rod, A supercritical fluid container and a liquid raw material tank are connected to the high-pressure reaction tank for supplying supercritical fluid and liquid raw material respectively, and the supercritical flow system is in a supercritical state carbon dioxide fluid; A plurality of high-pressure pumps are provided between the supercritical fluid container, the liquid raw material tank and the high-pressure reaction tank, and are used to pressurize and convey the supercritical fluid and liquid raw materials to the high-pressure reaction tank; and a plurality of control valves are respectively provided in the respective The supercritical fluid container, the liquid raw material tank and the high-pressure reaction tank are used to control the flow direction of the supercritical fluid, liquid raw material and extraction liquid, respectively. 如申請專利範圍第1項所述之高效率超音波萃取設備,其中,係包含有一第一高壓反應槽與若干第二高壓反應槽,該超臨界流體容器與液體原料罐係連接第一高壓反應槽之槽體頂端與底端,該第一高壓反應槽之槽體頂端、底端並透過二連接管合併後連接第二高壓反應槽之槽體頂端,用以可供該第一高壓反應槽內之萃取液再輸送至第二高壓反應槽進行萃取。The high-efficiency ultrasonic extraction equipment according to item 1 of the patent application scope, which comprises a first high-pressure reaction tank and a plurality of second high-pressure reaction tanks, and the supercritical fluid container and the liquid raw material tank are connected to the first high-pressure reaction. The top and bottom of the tank body of the tank, the top and bottom ends of the tank body of the first high-pressure reaction tank are combined through two connecting pipes and connected to the top of the tank body of the second high-pressure reaction tank, so that the first high-pressure reaction tank The extraction solution in the solution is sent to a second high-pressure reaction tank for extraction. 如申請專利範圍第2項所述之高效率超音波萃取設備,其中,該二連接管上並分別設有該控制閥。The high-efficiency ultrasonic extraction device as described in the second item of the patent application scope, wherein the two connecting pipes are respectively provided with the control valve. 如申請專利範圍第2項所述之高效率超音波萃取設備,其中,該超臨界流體容器與液體原料罐之輸出管路係合併後再連接第一高壓反應槽之槽體頂端、底端,各該輸出管路上分別設有該高壓幫浦。The high-efficiency ultrasonic extraction equipment as described in the second item of the scope of the patent application, wherein the supercritical fluid container and the liquid raw material tank output line are combined and then connected to the top and bottom ends of the tank of the first high-pressure reaction tank, The high-pressure pump is provided on each of the output pipelines. 如申請專利範圍第4項所述之高效率超音波萃取設備,其中,該超臨界流體容器與液體原料罐之輸出管路上更分別設有該控制閥,係介於各該高壓幫浦與第一高壓反應槽之槽體頂端、底端之間。The high-efficiency ultrasonic extraction equipment according to item 4 of the scope of the patent application, wherein the output valve of the supercritical fluid container and the liquid raw material tank is further provided with the control valve, which is located between the high-pressure pump and the first The top and bottom ends of a high-pressure reaction tank. 如申請專利範圍第2項所述之高效率超音波萃取設備,其中,該出料口上設有一控制閥。The high-efficiency ultrasonic extraction device as described in the second item of the patent application scope, wherein the discharge port is provided with a control valve. 如申請專利範圍第3、4、5或6項所述之高效率超音波萃取設備,其中,各該控制閥包含複數高壓閥、單向閥與若干背壓閥,各該高壓閥係分別設置於超臨界流體容器與液體原料罐之輸出管路、二連接管及各高壓反應槽之出料口,用以供控制該超臨界流體容器與液體原料罐之輸出壓力、啟閉及各高壓反應槽是否輸出萃取液,各該單向閥係分別設置於超臨界流體容器與液體原料罐之輸出管路及連接該第一高壓反應槽之槽體底端之連接管,用以防止加壓之超臨界流體與液體原料回流及防止該連接管內之萃取液朝第一高壓反應槽之槽體底端回流,該背壓閥係設置於連接該第一、第二高壓反應槽之槽體頂端之連接管,用以可控制該連接管所需壓力與流量。According to the high-efficiency ultrasonic extraction equipment described in the scope of patent application No. 3, 4, 5, or 6, each of the control valves includes a plurality of high-pressure valves, a check valve, and a plurality of back pressure valves, and each of the high-pressure valves is provided separately. The output pipeline, two connecting pipes and discharge outlets of each high-pressure reaction tank at the supercritical fluid container and the liquid raw material tank are used to control the output pressure, opening and closing, and various high-pressure reactions of the supercritical fluid container and the liquid raw material tank. Whether the tank outputs the extraction liquid, each one-way valve system is respectively arranged on the output pipeline of the supercritical fluid container and the liquid raw material tank and the connecting pipe connected to the bottom end of the tank body of the first high-pressure reaction tank to prevent pressurization. Supercritical fluid and liquid raw materials return and prevent the extraction liquid in the connecting pipe from flowing back to the bottom end of the tank of the first high-pressure reaction tank. The back pressure valve is arranged at the top of the tank connected to the first and second high-pressure reaction tanks. The connecting pipe is used to control the pressure and flow required by the connecting pipe. 一種提升超臨界萃取效率之方法,主要係於超臨界流體濕合液體原料進行萃取之過程中,同時對液體原料進行超音波振盪,以萃取、分離出對人體有益之營養成分,進而可提高該高壓反應槽之萃取效率、縮短萃取時間,其中,係於至少一高壓反應槽內進行萃取過程,該高壓反應槽一端連接有一超臨界流體容器與一液體原料罐,供將超臨界流體與液體原料混合後輸入高壓反應槽,該高壓反應槽包含開口朝上之一槽體,該槽體底端設有一出料口,供輸出萃取液,一蓋體,蓋設於該槽體之頂端開口,一超音波棒,設置於該蓋體內而伸入槽體。A method for improving supercritical extraction efficiency is mainly in the process of supercritical fluid wetted liquid raw material extraction, while ultrasonically oscillating the liquid raw material at the same time, in order to extract and separate nutritious components that are beneficial to the human body, thereby improving the The extraction efficiency of the high-pressure reaction tank and the shortening of the extraction time, wherein the extraction process is performed in at least one high-pressure reaction tank, and one end of the high-pressure reaction tank is connected with a supercritical fluid container and a liquid raw material tank for supercritical fluid and liquid raw materials. After mixing, it is input into a high-pressure reaction tank. The high-pressure reaction tank includes a tank body with an opening facing upward. The bottom end of the tank body is provided with a discharge port for outputting the extraction liquid. A cover body is arranged on the top opening of the tank body. An ultrasonic rod is arranged in the cover body and extends into the groove body. 如申請專利範圍第8項所述提升超臨界萃取效率之方法,其中,係包含有一第一高壓反應槽與若干第二高壓反應槽,該超臨界流體容器與液體原料罐係連接第一高壓反應槽之槽體頂端與底端,該第一高壓反應槽之槽體頂端、底端並透過二連接管合併後連接第二高壓反應槽之槽體頂端,用以可供該第一高壓反應槽內之萃取液再輸送至第二高壓反應槽進行萃取、分離。The method for improving supercritical extraction efficiency as described in item 8 of the scope of patent application, which comprises a first high-pressure reaction tank and a plurality of second high-pressure reaction tanks, and the supercritical fluid container and the liquid raw material tank are connected to the first high-pressure reaction. The top and bottom of the tank body of the tank, the top and bottom ends of the tank body of the first high-pressure reaction tank are connected through the two connecting pipes and connected to the top of the tank body of the second high-pressure reaction tank, so that the first high-pressure reaction tank can be used. The extracted liquid in the solution is sent to a second high-pressure reaction tank for extraction and separation.
TW107137111A 2018-10-19 2018-10-19 High-efficiency ultrasonic extraction equipment and method for improving supercritical extraction efficiency TWI680012B (en)

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