1351505 九、發明說明： 【發明所屬之技術領域】 法’尤指一種可加速 歇性微波加熱及控制 以提高欲乾燥樣品的 之時間及達到節能之 ，其概應隸屬於生物1351505 IX. Description of the invention: [Technical field to which the invention pertains] The law, in particular, refers to an accelerated microwave heating and control to increase the time required to dry a sample and achieve energy saving.
本發明係關於一種冷凍乾燥的方 冷康乾燥速率的有效方法，其係以間 冷凍乾燥過程中溫度及壓力的改變， 熱傳及質傳速率，藉以縮短乾燥所需 目的，並且不破壞欲乾燥樣品的活性 材料處理之技術領域範疇。 【先前技術】 按，一般冷凍乾燥的方 水份由凍結狀態直接昇華成 乾燥方法能夠得到高品質之 被使用於生物'醫藥及食品 性的乾燥方法。 法係在高度真空的條件下，將 氣態而除去的乾燥方法，此種 咼知值乾燥樣品，故而廣泛地 製造等方面，為具有相當實用 既有技術於冷；東乾燥拉The invention relates to an effective method for freeze-drying the drying rate of the square cold, which is characterized by the change of temperature and pressure during the freeze-drying process, the heat transfer and the mass transfer rate, thereby shortening the purpose of drying and not destroying the drying. The technical field of active material processing of samples. [Prior Art] According to the general freeze-dried water, it is directly sublimed from a frozen state to a dry method to obtain a high-quality drying method which is used for biological 'medicine and food. The method of drying the gas in a highly vacuum condition, such as drying the sample, so that it is widely manufactured, and is quite practical. The prior art is cold;
a , 時’ #先將欲乾燥的樣品急速Aa , time’ # first to dry the sample quickly A
凍，再把凍結的樣品置 τ 提供熱能給; 東結的樣。，固疋壓力的真空腔室内，並 表面在内逐步昇華成水蒸氣 由樣。。外 散出來而達到乾燥的效果…’，、乳由，東-的樣品中擴 進行加熱’ ·然而，由於樣乃可利用熱板熱傳導的方式 效率降低，而無法有效地：Γ孔狀的構造’容易使熱傳的 時Η具- "進订冷减乾燥’使得乾焊所需的 時間長，並且冷凍乾燥進行過 為“的 所需要的能量，同時又要 $ * S供冰結晶昇華 _ 0 要、准持真空及冷凍狀態，不僅合、、肖 耗大罝肊1而且不利於樣口 个惶a肩 樣。口的熱傳及質傳，相對增加冷;東 5 1351505 乾燥所需之成本。 因此，有人改變熱源的提供方式，利用微波技術來進 行加熱，其中應用微波的轄射熱源進行乾燥，雖然能夠縮 短約1/4〜1/3的乾燥所需時間，但是操作時連續性的微波 =射容易因微波能量分佈不均’容易產生樣品局部過熱的 致使乾燥後樣品的品，所^Μ能㈣ ^時間的情況下㈣又能達㈣能及提昇品質的效果， 係目前冷凍乾燥技術領域中所欲解決之問題。 【發明内容】 因此’本發明人有鑑於上述既有冷康乾燥技術於實際 用上的不足與問題，特經過不斷的研究與試驗，終於發 展出一種能改進現有缺失之本發明。 本發明之主要目的係在於提供-種加速冷凌乾燥速率 的有效方法，其係建立一個同時 ”、 统，科W Β π時包含屋力及溫度變化的系 統，對於壓力及溫度進行調節， 诘盅.隹品坦似 乂间樣。〇的熱傳及質傳 速率，進而美供一種可加速乾 省能源及降低成本之目的者 。樣—、即 知丁 進而將此種方法應用於食品 :、物活性樣品的保存及醫藥樣品上。 為達到上述目的’本發明係提供一 … 率的有效方法，I得以@„ ' σ、、凍乾燥速 知以微波間歇性加埶 狀態下進行真空乾燥，並摔 ；…於控制低溫 诛作步驟係包括如 (a )儀器裝置：揾 ^ 如i、一具減壓調節控制 波加熱功用之冷凍乾烊努署 』及間歇性裱 果导“裝置，其中該冷凍乾 -具腔室之本體、-與本體相連接的冷凝琴 莰7兮嘁35、—與冷凝器 6 I35l505 相連接的真空泵 控制模組及一設 、一設於冷凝器及真空栗 於本體内的間歇性微波模 之間的循環壓力 組； (b 樣品； 準儀樣品：製造準備進行冷綠燥的生物性材料 (c )降溫處理：將製備好的生物性材料樣品放於本體 的腔室内並透過冷凝器急速降溫至_4Gn東結至少 時； ，J、 ·")調節壓力：透過上述的真空泵對於本體的腔室進 行抽真空作業’待腔室呈現—真空狀態後，經由循環壓力控 制模組進行上、下限之絕對壓力； (e )加熱處理：待腔室内的壓力維持在所設定的上、 下限絕對壓力之間，啟動該間歇性微波模組，藉以對於樣品 進T間歇性加熱，使腔室内的壓力與溫度相配合調節，讓欲 乾燥樣品達到最佳的熱傳及質傳效率；以及 (f )進打乾燥：透過壓力調節與間歇性加熱的方式， •對於樣品進行乾燥處理。 車乂公地，於調節壓例的步驟中，將腔室内的絕對壓力 維持在〇· 1〜2mmHg之間。 車乂佳地，於加熱處理的步驟中，將微波模組的加熱溫 度设定為30〜4〇。〇之間。 較佳地，於加熱處理的步驟中，設定微波模組間歇性 加熱的猶環時間為20〜40分鐘。 争/J- | ’於加熱處理的步驟中，設定一間歇值 a =-^ίί_ y It rb T〇»+T〇ff ” f Γ。"為加熱及減壓至下限壓力之時間，而w為 7 1351505 ::加熱及壓力回復至上限壓力之時間，其中將該間歇值α設 - 疋為0.2〜0.9之間。 旦較佳地，於進行乾燥的步驟中，將樣品乾燥至水份含 • 為3 即元成樣品的冷凉乾燥處理。 . 藉由上述之技術手段，本發明加速冷康乾燥速率的有效 方法，係至少具有以下之優點及功效 一、冷凌乾燥速率：|發明透過壓力調節及微波間歇加 鲁…、的相互配合方式，可避免傳統利用微波連續性照射之冷 凍乾燥方法所具有的能量分佈不均及樣品局部過熱等缺 點，同時有效地增加熱傳及質傳的效率，可大幅縮短冷凉 乾燥所需之時間。 ,二、改善品質：本發明藉由間歇性微波模組的微波進 ^熱’不僅可直接穿透具多孔性結構之欲乾燥樣品，大 k门/、熱傳效率，且所用微波的能量較小，只能對於樣 。《產生熱效應，而不會使樣品產生化學變化，有效避免於 鲁乾燥過程中樣品的成分產生變化或因溫度過高而破壞樣品 活性，進而提供一較佳的乾燥品質。 ， 三、 節省能源：本發明可藉由循環壓力控制模組的操 作’對於腔室内的壓力進行調節及改冑，使腔室内的壓力 在-定區間值作改變，透過調整壓力大小的方式改變敎傳 及質傳的效率’藉以加速樣品的乾燥速率’進而達到節省 能源、降低成本及提昇產量之目的。 四、 適用性廣：本發明藉由微波進行加熱的方式，並將 加熱溫度設定在40〇C以下，可有效避免於乾燥過程中樣品 8 1351505 的成分產生變化或因温度過高而破壞樣品活性因此， 發明之冷凍乾燥方法可應用於例如：酵素、抗體、菌株本 細胞、組織等熱敏感性之生物性樣品上，進而提供—適、 性廣且符合市場需求之冷凍乾燥方法者。 $ 【實施方式】 為能詳細瞭解本發明的技術特徵及實用功效並可依 照說明書的内容來實施，玆進一步以圖式（如第一及-又 所示）所示的較佳實施例，詳細說明如后： 本發明之加速冷凍乾燥速率的有效方法，其主要係r 控制壓力調節及微波間歇性加熱的方式，在控制低溫的2 態下，於真空中達到加速乾燥之效果，其操作步驟包括如 下： ° 儀器裝置：提供一具減壓調節控制及間歇性微波加熱 功用之冷束乾燥裝置’其中該冷凍乾燥裝置係設有一具腔 室之本體（10)、一與本體（10)相連接的冷凝器（2〇)、一與冷 凝器（20)相連接的真空泵（30)、一設於冷凝器（2〇)及真空泵 (30)之間的循環壓力控制模組（4〇)及一設於本體（1〇)内的間 歇性微波模組； 準備樣品：製造準備進行冷凍乾燥的生物性材料樣品， 例如·加工食品、酵素、抗體、菌株、組織或藥品等； 降溫處理：將製備好的生物性材料樣品放於本體（丨〇)的 腔室内並透過冷凝器（20)急速降溫至_4(TC，並凍結至少24 小時； 調節壓力：透過上述的真空泵（3 0)對於本體（1〇)的腔室 9 1351505 進行拮真空作業，待腔室呈現一真空狀態後，經由循環壓力 控制柄組（40)進行上、下限之絕對壓力，使腔室内的壓 持在0.1〜2mmHg之間； 其中Γ<«為加熱及 力熱處理.凊參閱如第三圖所示，待腔室内的壓力維持 =所。又疋的上、下限絕對壓力之間，啟動該間歇性微波模組'， 錯以對於樣品進行間歇性的加熱’其中當壓力從上限絕對壓 力朝下限絕對壓力下降時，啟動該間歇性微波模組，對於樣 。口進仃持續加熱’待壓力下降至下限絕對壓力時則停止對 於樣品進行加熱，進而透過腔室内壓力與溫度相配合調節的 方式，讓欲乾燥樣品達到最佳的熱傳及質傳效率達到縮短 乾：：需時間及達到節能之效果，其中將微波模組的加熱： 2度二1广=之間，並設定該間歇性加熱的循環時間為 υ 刀I里，以及設宕一間歇值一 u , 減堡至下限壓力之時間，而〜為不加熱及塵力回復至上限壓 力之時間，其中將該間歇值α設定為〇.2〜0.9之間；以及 進行乾燥：透過上述壓力調節與間歇性加熱的方式，對 於樣品進行乾燥處理，使樣品乾駐水份含量為外 樣品的冷凍乾燥處理。 70 :由上述之技術手段’本發明可藉由間歇性微波模组 之^皮’不僅可直接穿透具多孔性結構之欲乾燥樣品，大 幅提南其熱傳效率，且微波的能量較小，只能對於樣。產 生熱效應，而不會使樣品產生化學變&，有_免於= :程：樣，的成分產生變化或因溫度過高而破壞樣品活 !·生秸以提供一適用範圍較廣的冷凍乾燥方式。 1351505 再則，本發明可藉由循環壓力控制模組（4〇)的操作， 對於腔室内的壓力進行調節及改變，使腔室内的壓力在/ 定區間值作改變，透過調整壓力大小的方式改變熱傳及質 傳的效率，藉以加速樣品的乾燥速率，因此，本發明可透 過間歇性微波模組與循環壓力控制組件（4 〇)的相互配合， 不僅可有效縮短樣品乾燥所需之時間，進而達到節省能 源、降低成本及提昇產量之目的，且透過微波加熱的方式， 可有效避免樣品於加熱過程中產生化學變化或破壞活性之 現象，因此，本發明之冷凍乾燥方法可應用於熱敏感性之 生物性樣品上’進而提供一適用性廣且符合市場需求之冷 康乾燥方法者。 【圖式簡單說明】 第一圖係本發明加速冷凍乾燥速率的有效方法之操作 第二圖係本發明加速冷凍乾燥速率的有效方法所使用 的冷凍乾燥裝置立體外觀示意圖。 第三圖係本發明加速冷凍乾燥速率的有效方法之壓力 與溫度之關係圖。 【主要元件符號說明】 (10)本體 (20)冷凝器 (30)真空泵 (40)循環壓力控制模組Freeze, then put the frozen sample to τ to provide heat energy; , the vacuum chamber of the solid pressure, and the surface gradually sublimes into water vapor. . It is released to achieve the effect of drying... ',, milk, and the sample in the east-heating is expanded'. However, since the sample is heat-transferable, the efficiency is lowered, and it is not effective: the pupil-like structure 'Easy to make the heat transfer time cooker - "booking cold reduction drying' makes the dry welding take a long time, and freeze-drying has been carried out as "the required energy, while at the same time $ * S for ice crystallization sublimation _ 0 It is necessary to hold the vacuum and the frozen state, not only the combination, but also the consumption of the 罝肊1 and it is not conducive to the shoulder of the sample. The heat transfer and quality of the mouth are relatively increased; the east 5 1351505 is required for drying. Therefore, some people change the way the heat source is supplied, and use microwave technology to perform heating. The microwave heat source is used for drying, although the drying time of about 1/4 to 1/3 can be shortened, but the operation is continuous. Sexual microwave = shot is easy due to uneven distribution of microwave energy 'prone to local overheating of the sample caused by the sample after drying, can be (4) ^ time (4) can reach (four) energy and improve the quality of the effect, is currently freezing The problem to be solved in the field of dry technology. [Summary of the Invention] Therefore, the present inventors have developed a kind of energy through continuous research and experiment in view of the above-mentioned deficiencies and problems in the practical use of the cold-drying technology. The present invention is directed to providing an effective method for accelerating the drying rate of cold chilling, which is to establish a system including house and temperature changes at the same time, for the system W Β π The pressure and temperature are adjusted, and the product is like a cockroach. The heat transfer and quality transfer rate of the cockroach, and the United States for a purpose to accelerate energy conservation and reduce costs. This method is applied to foods, storage of active samples and pharmaceutical samples. In order to achieve the above object, the present invention provides an effective method for the rate of I, @成', σ, freeze drying, vacuum drying under microwave intermittent twisting, and falling; The system includes, for example, (a) an instrument device: 揾^如i, a freeze-drying device for decompressing the control wave heating function, and an intermittent fruit-leaf device, wherein the body of the freeze-dry chamber has - a condensing hammer 7 兮嘁 35 connected to the body, a vacuum pump control module connected to the condenser 6 I35l505, and a set, a condenser, and a vacuum pump between the condenser and the intermittent microwave mold in the body Circulating pressure group; (b sample; quasi-meter sample: manufacturing biological material prepared for cold green drying (c) cooling treatment: placing the prepared biological material sample in the chamber of the body and rapidly cooling through the condenser to _ 4Gn East knot at least; , J, · ") Adjusting pressure: vacuuming the chamber of the body through the vacuum pump described above. 'When the chamber is presented—the vacuum state, the upper and lower sides are controlled by the circulating pressure control module. Absolute pressure; (e) Heat treatment: the pressure in the chamber is maintained between the set upper and lower absolute pressures, and the intermittent microwave module is activated, so that the sample is intermittently heated to make the pressure in the chamber Adjusted to match the temperature to achieve optimum heat transfer and mass transfer efficiency; and (f) dry drying: through pressure regulation and intermittent heating, • Drying the sample. In the step of adjusting the pressure, the absolute pressure in the chamber is maintained between 〇·1~2 mmHg. In the step of heat treatment, the heating temperature of the microwave module is set to 30 to 4 Torr. Between 〇. Preferably, in the step of heat treatment, the U-ring time for intermittently heating the microwave module is set to 20 to 40 minutes.争/J- | 'In the heat treatment step, set an intermittent value a =-^ίί_ y It rb T〇»+T〇ff ” f Γ." is the time to heat and depressurize to the lower limit pressure, and w is 7 1351505 :: heating and pressure return to the upper limit pressure, wherein the intermittent value α is set to - 疋 between 0.2 and 0.9. Preferably, in the step of drying, the sample is dried to moisture. The invention comprises: a cooling and drying treatment of a sample of 3 yuan. The above-mentioned technical means, the effective method for accelerating the drying rate of the present invention has at least the following advantages and effects: 1. The cold drying rate: Through the mutual adjustment of pressure regulation and microwave intermittent addition, the disadvantages of uneven distribution of energy and local overheating of the sample by the conventional freeze-drying method using microwave continuous irradiation can be avoided, and heat transfer and quality transfer are effectively increased. The efficiency can greatly shorten the time required for cooling and drying. Second, improve the quality: the microwave heating of the intermittent microwave module of the present invention can directly penetrate the porous sample with a porous structure, and the large sample k gate / The heat transfer efficiency, and the energy of the microwave used is small, can only be used for the sample. "Thermal effect is generated without chemical changes in the sample, effectively avoiding changes in the composition of the sample during the drying process or destroying the sample due to excessive temperature. The activity, in turn, provides a better drying quality. 3. Energy saving: The present invention can adjust and improve the pressure in the chamber by the operation of the circulating pressure control module, so that the pressure in the chamber is within a predetermined interval. The value is changed, and the efficiency of the rumor and quality transmission is changed by adjusting the pressure to 'accelerate the drying rate of the sample' to save energy, reduce costs and increase production. 4. Wide applicability: The present invention uses microwave By heating and setting the heating temperature below 40 〇C, it is possible to effectively avoid the change of the composition of the sample 8 1351505 during the drying process or to destroy the activity of the sample due to the excessive temperature. Therefore, the freeze-drying method of the invention can be applied to, for example, : Enzymes, antibodies, strains, cells, tissues, and other biological samples that are sensitive to heat, and then provide A freeze-drying method that is broad in scope and meets market demand. [Embodiment] In order to understand the technical features and practical effects of the present invention in detail and to implement according to the contents of the specification, further drawings are adopted (such as the first and the - Also shown is a preferred embodiment shown, as described in detail below: An effective method for accelerating the freeze-drying rate of the present invention, which is mainly a method of controlling pressure regulation and intermittent microwave heating, in the state of controlling low temperature 2 The effect of accelerating drying is achieved in a vacuum, and the operation steps thereof include the following: ° Instrument device: a cold beam drying device providing a pressure reducing adjustment control and intermittent microwave heating function, wherein the freeze drying device is provided with a chamber The body (10), a condenser (2〇) connected to the body (10), a vacuum pump (30) connected to the condenser (20), a condenser (2〇) and a vacuum pump (30) Circulating pressure control module (4〇) and an intermittent microwave module disposed in the body (1〇); preparing samples: manufacturing biological material samples ready for lyophilization, for example Processing food, enzymes, antibodies, strains, tissues or medicines; cooling treatment: placing the prepared biological material sample in the chamber of the body (并) and rapidly cooling to _4 (TC, through the condenser (20). And freeze for at least 24 hours; adjust the pressure: through the vacuum pump (30) above, the chamber 9 1351505 of the body (1〇) is vacuumed, and after the chamber is in a vacuum state, the handle is controlled by the circulating pressure (40). The absolute pressure of the upper and lower limits is such that the pressure in the chamber is between 0.1 and 2 mmHg; wherein Γ<« is heat and heat treatment. 凊 See the third figure, the pressure in the chamber is maintained. The intermittent microwave module is activated between the upper and lower absolute pressures of the crucible, and the sample is intermittently heated. The intermediate microwave mode is activated when the pressure drops from the upper limit absolute pressure to the lower limit absolute pressure. Group, for the sample. The enthalpy of the mouth is continuously heated. When the pressure drops to the lower limit absolute pressure, the heating of the sample is stopped, and the pressure and temperature are adjusted in the chamber to adjust the heat transfer and mass transfer efficiency of the sample to be dried. Dry:: It takes time and energy saving effect, in which the microwave module is heated: 2 degrees 2 1 wide = between, and the cycle time of the intermittent heating is set to υ knife I, and set a pause value u, the time from the minus to the lower limit pressure, and ~ is the time when the heating and the dust force return to the upper limit pressure, wherein the intermittent value α is set to be between 〇.2 and 0.9; and drying is performed: In the manner of intermittent heating, the sample is subjected to a drying treatment, and the dry moisture content of the sample is freeze-dried for the external sample. 70: According to the above technical means, the invention can not directly penetrate the porous sample with a porous structure by using the intermittent microwave module, and greatly improve the heat transfer efficiency of the microwave, and the microwave energy is small. , only for the sample. Produces a thermal effect without chemically changing the sample, and there is a change in the composition of the sample or the temperature is too high to destroy the sample! The straw is provided to provide a wide range of freezing. Drying method. 1351505 Furthermore, the present invention can adjust and change the pressure in the chamber by the operation of the circulating pressure control module (4〇), so that the pressure in the chamber changes in the interval value, and the pressure is adjusted. The efficiency of heat transfer and mass transfer is changed to accelerate the drying rate of the sample. Therefore, the present invention can effectively shorten the time required for sample drying through the interaction of the intermittent microwave module and the circulating pressure control component (4 〇). In order to save energy, reduce cost and increase production, and through microwave heating, the phenomenon that the sample is chemically changed or destroyed during heating can be effectively avoided. Therefore, the freeze-drying method of the present invention can be applied to heat. On sensitive biological samples, it provides a wide-ranging and market-friendly cold-drying method. BRIEF DESCRIPTION OF THE DRAWINGS The first drawing is an operation of an effective method for accelerating the freeze-drying rate of the present invention. The second drawing is a schematic perspective view of a freeze-drying apparatus used in an effective method for accelerating the freeze-drying rate of the present invention. The third graph is a plot of pressure versus temperature for an effective method of accelerating freeze-drying rates in accordance with the present invention. [Main component symbol description] (10) Main body (20) Condenser (30) Vacuum pump (40) Cyclic pressure control module