201134536 六、發明說明： 【發明所屬之技術領域】 提供-種多崎輕界讀萃取伽裝置 才曰種、〜合超臨界流體之固相、 置，並善且m%E 液相卒取與精餾功能之裝 並1固顧、狀萃取與細舰、㈣ 取與精顧魏、高減補之萃 〃 °卒 ϋ 0 錢與刀離功能等多重用途與201134536 VI. Description of the invention: [Technical field to which the invention belongs] Provides a kind of multi-salt light-bound reading extraction gamma device, a solid phase of the supercritical fluid, and a good and m%E liquid phase pumping and The rectification function is packed with 1 solid, extracted and fine ship, (4) taken and refined, and the high-reduction of the 〃 ° ϋ 0 money and knife function and other purposes
【先前技術】 ^ m然、物或中草藥提取活性成分的方法包括榨磨 -^、水錢蒸躲、有機關浸提法和吸等。傳統上大 4用設備絲最低、操作最容易的水航難法來獲得。 ^查:水減_法溫度高又有水存在，容易導致熱敏性成 • t較熱分解、水解和水溶作科發生，降低產量和產物的 質而揮么11/合劑，文提法雖可降低提取溫度，但卻有溶劑 1殘留叹歸點成麵失的缺點。耻，後來财接近室溫 操作的超臨界流辟取妹代傳辭取方法成絲想替代方 法。 目前可使用的超臨界流體包括二氧化碳、找、乙烧、 丙院、乙稀、㈣等，其中又以二氧化碳最被普遍使用。超 b界二氧化碳流體為—種優良溶劑，具有低表面張力、低黏 201134536 度、無毒、便宜、容#取得、不燃、化學性質安定、不與萃 取物質發生反應等優點。由於其臨界溫度(31.rc)與臨界壓力 (72.8咖)均不高，因此應用在天然物萃取時，具有無溶劑殘 留、安全、製程簡單、萃取時間短、適用於熱不穩定成份取 得等優點，因而被廣泛地應用在天然物付效成分的提取。 而近年來更發展-種超臨界_精峨術，該技術除了 保留超臨界流體-貫的優點’更可在較低溫度下以溶解度的 差異性來分離沸點接近的化合物。 習知超臨界流鮮取與精健合之裝置，依原料狀態可 分為固相與液相_，第—圖為固相原料之萃取與精顧裝置 10，適合固體原料之萃取，先將JU體原料置人萃取槽1〇1中， 超臨界流體經過萃取槽101溶解原料中脂溶性成分後攜出， 再、·、呈過精顧官柱102進行特定成分之分離後，經過降壓而在 分離槽103獲得低滞點組份與氣態流體，氣態流體經過冷凝 後成為液體而儲放於儲存槽1〇4内，以供回收再使用。另在 精館s柱1〇2底部獲得面沸點組份，因而達到分離與濃縮效 果。 第二圖為液相原料之萃取與精織置20，適合高黏度液 體之萃取。先將液相原料導入底部萃取槽2m，超臨界流體經 過萃取槽201岭解原料中脂溶性成分後攜出，向上經過精顧 201134536 官柱202進行特定成分之分離後，經過降壓而在分離槽期 獲得低沸點組份，而萃取槽2〇1内則留下高彿點組份。 第三圖為適合低減液體之逆向萃取裝置3Q，令原料槽 301内之液相原料自精鮮柱3G2上段或中段進人後自底部排 出’令超臨界流體供應單元3〇3之超臨界流體自精顧管柱3〇2 ' 底部進入後自頂端排出。當兩種流^在精顧管柱302内對流 籲 綱以後’超臨界流體將溶解液相原料中的脂溶性成分後攜 出，經過降壓而在分離槽304獲得低沸點組份。 惟，上述習知超臨界流體萃取與精鶴整合之裝置，會因 ' 原料狀態為固相或液相之差異而有不同的裝置設計，對於多 - 樣態原料之萃取與精餾操作，實際上具有設備投資成本高、 空間需求大等缺點。 ^ 有鑑於此，本發明人特地針對習知超臨界流體萃取與精 顧整合之裝置加以研究及改良，並在經過不斷測試及改良後 有本發明問世。 【發明内容】 緣是，本發明之目的在解決傳統超臨界流體萃取與精餾 整合之裝置具有設備投資成本高，及空間需求大之問題。 本發明主要係提供一種多用途超臨界流體萃取精餾裝 201134536 出口’内部有填充物，外部有加::少:個:上之流體進 至少-個以上之流體進出口，頂 底部連結。 頂相快開機構與該精顧管柱 -種多崎超臨錯群取精餾 精餘管柱，具註少-個-之流體進“含充物一 外部有加熱絲；- 口，頂部以快開機構與該崎柱底部 ：= ==，該祕包含崎路輸送該超臨界流體至該萃_ :=氣體槽’且管路上設有增壓幫浦與熱交換器以分 別對该越加顯加熱；—分_，財至少—偏上之流 體進出口’用來分離該流體與萃取物；及-壓力控制闊，位 於該精減該分_之間，用來控_精餾管柱與該萃 取槽内之壓力。 據上所述之多騎超臨界流鮮取精難置，其中，該 裝置係s、、且液相原料供應彳、統，該彡統包含以管路輸送 該液相原料·精㈣桂之液態原觸，且管路上設有增屢 泵浦與控制閥，以分別加壓及控制輸送量。 據上所述之多用途超臨界流體萃取精館裝置，其中，該 填充物係為铺峨質或為喊材成之填充物。 201134536 據上所述之多用途超臨界流鮮取精鮮置，其中，該 快開機構為夾鉗式快開機構。 —據上所述之多用途超臨界流體萃取精_置，其中，該 萃取槽内部設有—活動式氣體分散器。 據上所述之多用途超臨界流體萃取精餾裝置，其中，該 萃取槽内部設有一活動式内槽。 據上所述之多用途超臨界流體萃取精鋪置，其中，該 内槽並設置有過濾裝置。 藉以上设置’本發明她於習知超臨界流鮮取與精顧 ^ &之裝1· i要具有可適用於不同組態原料之萃取與精 德、降低賴投减本、提昇萃取效率、避免原料阻塞、操 作容易，及易於清洗等優點與功效。 【實施方式】 關於本創作人之技術手段，兹舉數讎佳可行實施例配 合圖式於下文進彳了詳細說明，俾供鈞上深人了解並認同本 創作。 請參閱第四圖所示’本發明具體實施例之主要結構包含 精條管枉1與卒取槽2，其中： 201134536 辭柱1可為多段式設計，且設有—超臨界流體出 口厂多她相原料人口 12’該等超臨界流财σ u與液 =原料入D U係分別設置在精崎柱丨之上巾下各段，精顧 :柱1内部設有獨鋪或喊製軌物u，軸管柱1外 部設有加熱絲14，用啸制各段溫度職自下而上遞增之 溫度梯度； 该萃取槽2位於精鮮柱丨下方，並以錢式快開機構 21々與精餾諸丨底部賴，使萃取槽2之槽财快速脫離精 德、s柱1，並藉由滑動與移載機構（圖未綠示）可使槽體升降 與平移’使_原料、高黏度液相原料之裝填、卸載操作更 加容易’並胁清洗；又，該萃取槽2底部設有—超臨界流 體入口 22(該超臨界越人σ 22除可設置料輯2底部以 外亦可選擇設置在萃取槽2的側邊）與一液相原料出口 ^， 萃取槽2外部亦設有加熱夾套24。 以上所述之具體實施例係適用於低黏度液體之逆向萃 取。另當上述具體實施例翻在高黏度液械料之萃取與精 鶴時’卿進-步在萃取槽2内底部設置活動式之氣體分散 益3 ’如第五、六圖所示，本發明之氣體分散器3係成型具有 輻射狀官路31與傾斜開孔32，絲將超臨界流體沿徑向分散 成夕股氣流，並可在經賴斜開孔32時形成小氣泡並產生渴 流’增加超臨界流體與原料的接觸面積以提升萃取效率。而 201134536 第七圖所7F則疋本發明具體實關相於難原料之萃取與 精德其主要係在萃取槽2内設有可裝填粉碎細體原料之 活動式内槽4 ’該内槽4上下端均設有網狀或燒結的或纖維的 過濾'裝置41，以防止_原料之微細顆粒進人精㈣柱u 萃取槽2内造成阻塞。 /、 此外，本伽之具體實施例可進—步搭配—組超臨界户 體供應系統5，請參閱第簡所示，該系統包含液化氣L 邮1’該壓縮液化氣體槽51以管路連接萃取槽2之超帥 流體入口 22，且管路上·^古描两 1 路上4增觀浦52及熱交換器幻 熱;一分離槽6，以管路連接_ 及一虔雜入口 U ’用以分離該臨界流體與萃取物，· 上= 精館管柱1與分離槽6之間的管路 上’用來控制精館管柱！與萃取槽2内雜力。 再者，關於本發明用以裝填固相原料 之方式，除可如前述操作令 …夜相原料 以後再進概填以外，亦：：^2體_精顧管柱1 系統8 (同如第八圖所示）， 、 、而夜相原料供應 液_槽81分別以管路連接各精槽81，該 ⑴且管路上設魅 娜目原料入口 加壓及控·送量，域 以刀別對液相原料[Prior Art] ^ The method of extracting the active ingredient from the product, or the Chinese herbal medicine, includes extracting -^, water money, steaming, organ extraction and suction. Traditionally, it is obtained by the method of water navigation that is the lowest and the easiest to operate. ^Check: water reduction _ method temperature is high and there is water, it is easy to cause heat sensitivity to become more thermal decomposition, hydrolysis and water dissolution, reducing the yield and quality of the product and the 11 / mixture, although the text can be reduced The temperature is extracted, but there is a disadvantage that the residual residue of the solvent 1 is lost. Shame, later the money approached the room temperature operation of the supercritical streamlined approach to the sister-generation method of resignation into a silk alternative. Currently available supercritical fluids include carbon dioxide, sulphur, sulphur, propylene, ethene, (iv), etc., of which carbon dioxide is most commonly used. The super-b boundary carbon dioxide fluid is an excellent solvent with low surface tension, low viscosity, 201134536 degrees, non-toxic, cheap, volumetric, non-flammable, chemically stable, and does not react with extracted materials. Because its critical temperature (31.rc) and critical pressure (72.8 coffee) are not high, it has no solvent residue, safe, simple process, short extraction time, suitable for heat unstable components, etc. The advantages are thus widely used in the extraction of natural ingredients. In recent years, there has been a development of supercritical _ fine sputum, which not only retains the advantages of supercritical fluids, but also separates compounds with similar boiling points at lower temperatures with solubility differences. The device for supercritical fresh-flow and fine-mixing can be divided into solid phase and liquid phase according to the state of raw materials. The first figure is the extraction and purification device 10 of solid phase raw materials, which is suitable for the extraction of solid raw materials. The raw material is placed in the extraction tank 1〇1, and the supercritical fluid is dissolved by the fat-soluble component in the raw material through the extraction tank 101, and then is separated from the specific component by the fine-grained column 102, and then depressurized in the separation tank. 103 obtains a low stagnation component and a gaseous fluid, and the gaseous fluid is condensed to become a liquid and stored in the storage tank 1〇4 for recycling. In addition, the boiling point component of the surface was obtained at the bottom of the column 1〇2 of the Jingsuo column, thus achieving the separation and concentration effect. The second picture shows the extraction and fine weaving of liquid phase materials, which is suitable for the extraction of high viscosity liquids. First, the liquid phase raw material is introduced into the bottom extraction tank 2m, and the supercritical fluid is taken out through the extraction tank 201 to dissolve the fat-soluble component in the raw material, and then taken up through the separation of the specific components of the 201134536 official column 202, and then separated by depressurization. The low boiling point component is obtained in the trough period, while the high Buddha point component is left in the extraction tank 2〇1. The third figure is a reverse-extraction device 3Q suitable for low-liquid reduction, so that the liquid phase raw material in the raw material tank 301 is discharged from the bottom portion or the middle portion of the refined fresh column 3G2, and the supercritical fluid of the supercritical fluid supply unit 3〇3 is discharged from the bottom. Since the bottom of the column 3〇2', the bottom is discharged and discharged from the top. When the two streams are convected in the string 302, the supercritical fluid will be dissolved after dissolving the fat-soluble component in the liquid phase material, and a low-boiling component is obtained in the separation tank 304 by depressurization. However, the above-mentioned conventional device for supercritical fluid extraction and integration of fine cranes has different device designs due to the difference in the state of the raw material as a solid phase or a liquid phase, and actually has an extraction and rectification operation for the multi-form material. The equipment has high investment cost and large space demand. In view of the above, the inventors have studied and improved the conventional supercritical fluid extraction and sophisticated integration devices, and have been subjected to the present invention after continuous testing and improvement. SUMMARY OF THE INVENTION The reason is that the object of the present invention is to solve the problem of high equipment investment cost and large space demand in the conventional supercritical fluid extraction and rectification integration device. The invention mainly provides a multi-purpose supercritical fluid extractive distillation apparatus 201134536. The outlet has internal fillings, and the external ones are added:: less: one: the upper fluid enters at least one or more fluid inlets and outlets, and the top and bottom are connected. The top phase quick opening mechanism and the intensive tube column - the species of the multi-small super fault group take the rectification of the remaining tube column, with a less---the fluid into the "filling with an external heating wire; - mouth, top With a quick opening mechanism and the bottom of the slate column: ===, the secret contains the supercritical fluid to the extraction _:=gas tank' and the pipeline is provided with a booster pump and a heat exchanger to respectively The more obvious heating; - _, 财 at least - upper fluid inlet and outlet 'used to separate the fluid and extract; and - pressure control is wide, located between the refined _, used to control _ rectification The pressure in the column and the extraction tank. According to the above, the riding of the supercritical stream is difficult to set, wherein the device is s, and the liquid phase raw material is supplied to the system, and the system includes the pipeline. The liquid raw material and the fine liquid of the liquid material are conveyed, and the pump is provided with an additional pump and a control valve to pressurize and control the conveying amount respectively. According to the multi-purpose supercritical fluid extraction and fine museum device described above Wherein, the filling is a screed or a filling material. 201134536 According to the multi-purpose supercritical fresh-keeping Wherein, the quick opening mechanism is a clamp type quick opening mechanism. - According to the multi-purpose supercritical fluid extraction method described above, wherein the extraction tank is internally provided with a movable gas disperser. The multi-purpose supercritical fluid extractive distillation apparatus, wherein the extraction tank is internally provided with a movable inner tank. According to the multi-purpose supercritical fluid extraction finishing device described above, the inner tank is provided with a filtering device. By the above setting, the invention is based on the conventional supercritical fluid extraction and the fineness of the ^^. Avoid the advantages of raw material blockage, easy operation, and easy cleaning. [Embodiment] Regarding the technical means of the creator, a detailed description of the feasible embodiments and the drawings is provided below. The person understands and agrees with the creation. Please refer to the fourth figure. The main structure of the embodiment of the present invention includes the fine tube 枉1 and the stroke groove 2, wherein: 201134536 The column 1 can be a multi-stage design, and It is equipped with a supercritical fluid export factory and more than 12% of its raw material population. These supercritical fluids σ u and liquid = raw materials into the DU system are set separately under the submerged section of the Seisaki column. There is a sole or shouting rail u, and a heating wire 14 is arranged outside the shaft column 1, and the temperature gradient from the bottom to the top of each temperature is used to make the temperature rise; the extraction tank 2 is located below the fine column, and With the money-type quick-opening mechanism 21々 and the bottom of the distillation column, the trough of the extraction tank 2 is quickly separated from the Jingde and S-pillars 1, and the trough body can be made by the sliding and transfer mechanism (not shown). Lifting and translating 'making the loading and unloading of raw materials, high-viscosity liquid raw materials easier and preventing the cleaning"; further, the bottom of the extraction tank 2 is provided with a supercritical fluid inlet 22 (the supercritical surrogate σ 22 can be removed) In addition to the bottom of the set 2, the side of the extraction tank 2 may be optionally disposed with a liquid phase material outlet, and the heating jacket 24 is also provided outside the extraction tank 2. The specific embodiments described above are applicable to the reverse extraction of low viscosity liquids. In addition, when the above specific embodiment is turned over in the extraction and sharp crane of the high-viscosity liquid mechanical material, the liquid gas dispersion of the movable type is set in the bottom of the extraction tank 2 as shown in the fifth and sixth figures. The gas disperser 3 is formed with a radial path 31 and a slanted opening 32. The wire disperses the supercritical fluid radially into a tidal stream, and forms small bubbles and generates a thirsty flow when the hole 32 is slanted. 'Increase the contact area of the supercritical fluid with the raw material to improve the extraction efficiency. In the seventh section of 201134536, the 7F of the present invention is specifically related to the extraction of difficult raw materials and Jingde. The main purpose is to provide a movable inner tank 4 in the extraction tank 2 which can be filled with pulverized fine raw materials. Both the upper and lower ends are provided with a mesh or sintered or fiber filtration device 41 to prevent the fine particles of the raw material from entering the fine (4) column u to cause clogging in the extraction tank 2. In addition, the specific embodiment of the present gamma can be further combined with the group of supercritical household supply system 5, as shown in the simplified embodiment, the system includes liquefied gas L mail 1 'the compressed liquefied gas tank 51 is pipelined Connected to the super handsome fluid inlet 22 of the extraction tank 2, and on the pipeline, the two towers on the road 1 and the heat pump magic heat; a separation tank 6, connected by a pipe _ and a noisy inlet U ' Used to separate the critical fluid and the extract, · on the pipe between the fine column 1 and the separation tank 6 'used to control the fine column! With the extraction tank 2 internal friction. Furthermore, as for the method for loading the solid phase raw material of the present invention, in addition to the above-mentioned operation order, the night phase raw material is further filled in, and also:: 2 body _ careful care column 1 system 8 (the same as the first In the eighth figure, the night phase raw material supply liquid_slot 81 is connected to each of the fine grooves 81 by a pipeline, and the (1) and the pipeline are provided with the inlet and pressure of the charm material inlet, and the field is cut. Liquid phase raw material
中。 字液相原料輸送進入精餾管柱I 9 201134536 藉以上設置，本發明可具有以下功效及優點： 1. 適用性佳.可彈性適㈣相或液相原料之萃取與精顧。 2. 降低成本：具有固相原料萃取與精餘、高黏度液相原 料之萃取與_、絲度㈣之勒萃取多重魏，降低設 備投資成本。 3. 特殊氣體分散器用在高黏度液相原料萃取，提高超臨 界流體與原料接觸面積以提升萃取效率。 4. 可避免ϋ相原料造雜塞：特軸槽用如相原料萃 取秦碎之固相原料裝填在内槽中，再將内槽置入萃取槽内， 可避免固體粉末進入精餾管柱造成阻塞。 操作方便胃於清洗·夾鉗式快開機構連結萃取槽與 精顧管柱，萃取射無鮮㈣速分離，使_原料、高、 黏度液相顧H卸鏡作容易，並祕清洗。 ’ π上所述’本翻賴露之技術手段確可達致職之目的 與功效且具長遠進步性，誠屬可供產業上利用之發明無誤，妥 依法提出申明，懇;y斤鈞上惠予詳審並賜准發明專利，至感德 馨。 —惟社所述者’僅為本發明之較佳實施例，當不能以此限 —發月實施之範圍’即大凡依本發明申請專利範圍及發明說 201134536 明書内容所作之等效 範圍内。 變化與修•’皆應仍屬本發明專利涵蓋之 【圖式簡單說明】 第一圖係習知_原料之萃取與精置示意圖。 第二圖係習知液相原料之萃取與精錄置示意圖。 第二圖係習知低黏度液體之逆向萃取裝置示意圖。 第四圖係本發明之精餾管柱鮮取槽之具體實細示意圖。 第五圖係本發明之萃取槽設置氣體分散器之示意圖。 第六圖係本發明氣體分散器之結構示意圖。 第七圖係本發明之萃取槽設置内槽之示意圖。 第八圖係本發明另一具體實施例之使用狀態示意圖。 【主要元件符號說明】 【習知部份】 10-萃取與精餾裝置 ιοί-萃取槽 102〜精餾管柱 103-分離槽 1G4--儲存槽 20-萃取與精餾裝置 201134536 201-萃取槽 202--精餾管柱 203-分離槽 30--逆向萃取裝置 301-原料槽 302--精餾管柱 303--超流體供應單元 【本發明】 304--分離槽 1--精餾管柱 11--超臨界流體出口 12-液相原料入口 13--填充物 14--加熱夾套 2-萃取槽 21--快開機構 22--超臨界流體入口 23-_液相原料出口 24--加熱夾套 3-氣體分散器 31-管路 32-開孔 4-内槽 41--過濾裝置 5--超臨界流體供應系統 51-壓縮液化氣體槽 52-增壓泵浦 53--熱交換器 6--分離槽 12 201134536 8--液相原料供應糸統 7--壓力控制閥 81 --液態原料槽 82--增壓泵浦 83--控制閥in. The liquid phase raw material is transported into the rectifying column I 9 201134536 By the above arrangement, the invention has the following functions and advantages: 1. Applicability is good. The elastic and suitable (four) phase or liquid phase raw material extraction and fineness. 2. Reduce costs: with solid phase raw material extraction and fine, high viscosity liquid phase raw material extraction and _, silk (4) extract multiple Wei, reduce equipment investment costs. 3. The special gas disperser is used for high viscosity liquid phase extraction to improve the contact area between the supercritical fluid and the raw material to improve the extraction efficiency. 4. It can avoid the plugging of the raw material of the ϋ phase: the special shaft tank is filled with the solid phase raw material of the phase raw material, and the inner tank is placed in the extraction tank to prevent the solid powder from entering the distillation column. Causes blocking. Easy to operate, the stomach is cleaned, the clamp-type quick-opening mechanism is connected to the extraction tank and the tube is carefully taken care of, and the extraction shot is fresh (four) speed separation, so that the raw material, the high-viscosity liquid phase is easy to remove the mirror, and the secret is cleaned. 'The above-mentioned technical means of π 上 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露 露Hui will give a detailed examination and grant a patent for invention, to the sense of Dexin. - the only part of the present invention is 'only the preferred embodiment of the present invention, and the scope of the implementation of the invention is not limited to the extent of the implementation of the invention", that is, within the equivalent range of the contents of the patent application and the invention of 201134536 . The changes and repairs should be covered by the patents of the present invention. [The simple description of the drawings] The first figure is a schematic diagram of the extraction and finishing of raw materials. The second figure is a schematic diagram of the extraction and purification of the liquid phase raw materials. The second figure is a schematic diagram of a conventional reverse extraction apparatus for low viscosity liquids. The fourth figure is a detailed schematic diagram of the fresh-drawn trough of the rectifying column of the present invention. The fifth drawing is a schematic view of the extraction tank setting gas disperser of the present invention. Figure 6 is a schematic view showing the structure of the gas disperser of the present invention. The seventh drawing is a schematic view showing the arrangement of the inner tank of the extraction tank of the present invention. Figure 8 is a schematic view showing the state of use of another embodiment of the present invention. [Main component symbol description] [Learn part] 10-extraction and rectification apparatus ιοί-extraction tank 102~ rectification column 103-separation tank 1G4--storage tank 20-extraction and rectification apparatus 201134536 201-extraction tank 202--rectification column 203-separation tank 30--reverse extraction device 301-feed tank 302--refrigerating column 303--super fluid supply unit [present invention] 304--separation tank 1--reflow tube Column 11 - Supercritical Fluid Outlet 12 - Liquid Phase Feedstock Inlet 13 - Filler 14 - Heating Jacket 2 - Extraction Tank 21 - Quick Opening Mechanism 22 - Supercritical Fluid Inlet 23 - Liquid Phase Material Outlet 24 - Heating jacket 3-gas disperser 31 - Line 32 - Opening 4 - Inner tank 41 - Filtration device 5 - Supercritical fluid supply system 51 - Compressed liquefied gas tank 52 - Boost pump 53 - Heat exchanger 6 - Separation tank 12 201134536 8--Liquid raw material supply system 7 - Pressure control valve 81 - Liquid material tank 82 - Booster pump 83 - Control valve
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