JP6933338B2 - Thermal decomposition treatment device for the object to be processed and thermal decomposition treatment method for the object to be processed - Google Patents
Thermal decomposition treatment device for the object to be processed and thermal decomposition treatment method for the object to be processed Download PDFInfo
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Description
本発明は植物等の被処理物の熱分解処理装置および被処理物の熱分解処理方法に関する。 The present invention relates to a thermal decomposition treatment apparatus for an object to be treated such as a plant and a method for thermal decomposition treatment of the object to be treated.
発明者は先に、植物組織中の有効成分抽出方法を開発している（特許文献１：特開２０１２−１９７１３号公報）。
この植物組織中の有効成分抽出方法は、植物原料を被処理物として密閉空間内で、密閉空間内の分圧として水蒸気圧を飽和水蒸気圧曲線に沿って制御しつつ植物組織の加水分解に必要な圧力と温度である温度１２５℃〜１３５℃、圧力を２気圧〜３気圧の範囲で一定時間その圧力、温度を保ち、その後、飽和水蒸気圧曲線に沿って圧力及び温度を制御しつつ密閉空間内の温度及び圧力を下降させ、密閉空間内に発生する水蒸気を植物組織内に浸透させて植物組織を加水分解するとともに、密閉空間内の水蒸気圧を被処理物の表面に作用させ、加水分解によって生成した植物組織内成分を被処理物の外部に搾り出す処理である。
The inventor has previously developed a method for extracting an active ingredient in a plant tissue (Patent Document 1: Japanese Patent Application Laid-Open No. 2012-19713).
This method for extracting the active ingredient in the plant tissue is necessary for the hydrolysis of the plant tissue while controlling the water vapor pressure along the saturated water vapor pressure curve as the partial pressure in the closed space in the closed space using the plant raw material as the object to be treated. The pressure and temperature are 125 ° C to 135 ° C, and the pressure is maintained in the range of 2 to 3 atm for a certain period of time, and then the closed space is controlled while controlling the pressure and temperature along the saturated water vapor pressure curve. The temperature and pressure inside are lowered, and the water vapor generated in the closed space permeates into the plant tissue to hydrolyze the plant tissue, and the water vapor pressure in the closed space acts on the surface of the object to be treated to hydrolyze. This is a process of squeezing the components in the plant tissue produced by the above method to the outside of the object to be treated.
主な植物組織成分を含む蒸気の温度・圧力域では、飽和水蒸気圧より少しでも温度が高いと炭化し、低いと不完全分解による不純物の液化混入の危険が生ずる。そこで、圧力容器内の雰囲気の温度と、圧力とをコンピューター制御によって、微妙な温度・圧力域を維持する。圧力容器内を飽和水蒸気圧曲線上の温度ｔを１２５℃以上、１３５℃以下、２〜３気圧の範囲に維持することによって、水蒸気が被処理物の組織内に深く浸透して組織の分解を促進する。 In the temperature and pressure range of steam containing the main plant tissue components, if the temperature is even slightly higher than the saturated steam pressure, it will be carbonized, and if it is lower, there is a risk of liquefaction of impurities due to incomplete decomposition. Therefore, the temperature and pressure of the atmosphere inside the pressure vessel are controlled by a computer to maintain a delicate temperature and pressure range. By maintaining the temperature t on the saturated water vapor pressure curve in the pressure vessel within the range of 125 ° C or higher, 135 ° C or lower, and 2 to 3 atm, water vapor penetrates deeply into the structure of the object to be treated and decomposes the structure. Facilitate.
上記特許文献１に示される熱分解処理方法は、色差分解処理といわれるものであり、水分子のブラウン運動の方向と位相を色力学的に整えてやることによって、水分子の連鎖に突然ウェーブが起こり、これが強大な破壊力となって、生体高分子のグリコシド結合を物理的に分断するという仕組みを利用している。この場合に重要なことは、これら高分子の構造水となっている水分子が飽和水蒸気圧の条件下で有効に働くということであり、圧力が飽和水蒸気圧点より低くても、また温度が飽和水蒸気圧点より高くても、水分子は高分子の構造から離れ、高分子は動きを止めてしまうため、分解処理ができなくなってしまう。 The thermal decomposition treatment method shown in Patent Document 1 is called a color difference decomposition treatment, and by chromatically adjusting the direction and phase of Brownian motion of water molecules, a wave suddenly appears in the chain of water molecules. It occurs, and this becomes a powerful destructive force, using a mechanism that physically breaks the glycosidic bond of biopolymers. What is important in this case is that the water molecules that are the structural water of these polymers work effectively under the condition of saturated water vapor pressure, and even if the pressure is lower than the saturated water vapor pressure point, the temperature is also high. Even if it is higher than the saturated water vapor pressure point, the water molecules move away from the structure of the polymer and the polymer stops moving, so that the decomposition treatment cannot be performed.
特許文献１に示される方法によれば、上記処理を行うことによって、植物の細胞組織、特に細胞壁に含まれる抗酸化成分や各種の有用成分を容易に、効率よく取り出すことができる。
ところで、特許文献１のものでは、圧力容器内の雰囲気の温度と、圧力とをコンピューター制御によって、微妙な温度・圧力域を維持するものであるが、圧力容器内の温度、圧力を飽和水蒸気圧曲線に沿うように制御することは必ずしも容易ではない。
According to the method shown in Patent Document 1, by performing the above treatment, the antioxidant component and various useful components contained in the cell tissue of the plant, particularly the cell wall, can be easily and efficiently taken out.
By the way, in Patent Document 1, the temperature and pressure of the atmosphere in the pressure vessel are controlled by a computer to maintain a delicate temperature / pressure range, but the temperature and pressure in the pressure vessel are saturated steam pressure. It is not always easy to control the pressure along a curve.
特に、特許文献１のものでは、ヒーターによる加温開始時に、電磁弁を閉じて圧力容器内を密閉するようにしている。このため、圧力センサで検出される圧力が、飽和水蒸気分圧と空気分圧の和となり、飽和水蒸気分圧を正確に検出することが困難となり、飽和水蒸気圧曲線に沿うように圧力容器内の温度、圧力を制御することが困難となる。
また、特許文献１のものでは、圧力容器内の水の沸騰を抑えることは考慮していない。特に、特許文献１のものでは、温度下降時（冷却時）に、圧力容器内の温度が、１２５℃以下に低下したときに電磁弁を開けているため、圧力容器内の水が沸騰しやすい。圧力容器内の水が沸騰すると、高分子を取り巻いている水の分子（構造水）が高分子から離れ、それぞれバラバラな分子となって勝手に動きまわるため、上記大きな破壊力（ウェーブ）が形成されなくなる。
In particular, in Patent Document 1, the solenoid valve is closed to seal the inside of the pressure vessel at the start of heating by the heater. Therefore, the pressure detected by the pressure sensor is the sum of the saturated water vapor partial pressure and the air partial pressure, making it difficult to accurately detect the saturated water vapor partial pressure, and the pressure inside the pressure vessel is along the saturated water vapor pressure curve. It becomes difficult to control the temperature and pressure.
Further, in Patent Document 1, it is not considered to suppress boiling of water in the pressure vessel. In particular, in Patent Document 1, since the solenoid valve is opened when the temperature in the pressure vessel drops to 125 ° C. or lower when the temperature drops (cooling), the water in the pressure vessel tends to boil. .. When the water in the pressure vessel boils, the water molecules (structural water) surrounding the polymer separate from the polymer and move around as separate molecules, forming the above-mentioned large destructive force (wave). Will not be done.
そこで本実施の形態は、上記課題を解決すべくなされたものであり、その目的とするところは、熱分解処理中に水の沸騰するのを回避し、圧力容器内の温度、圧力を飽和水蒸気圧曲線に沿って上昇、下降するよう制御することのできる被処理物の熱分解処理装置および被処理物の熱分解処理方法を提供することにある。
上記の目的を達成するため、本実施の形態は次の構成を備える。
すなわち、本実施の形態に係る被処理物の熱分解処理装置は、圧力容器と、該圧力容器を開閉する蓋体と、前記圧力容器内の温度を検出する温度センサと、前記圧力容器内の圧力を検出する圧力センサと、前記圧力容器を大気に開放可能な電磁弁と、前記圧力容器内を加温するヒーターと、前記温度センサにより検出される温度データおよび前記圧力センサにより検出される圧力データが入力され、該データに基づいて、前記ヒーターの出力を制御すると共に、前記電磁弁を開閉制御して、前記圧力容器内温度を１２５℃〜１４９℃にまで上昇させて、前記圧力容器内に収容した植物原料を被処理物として熱分解処理する制御部を有する被処理物の熱分解処理装置において、前記制御部は、前記ヒーターをオンして前記圧力容器内を加温する際、および前記ヒーターをオフして前記圧力容器内を冷却する際、前記圧力容器内の水を沸騰させることなく、かつ飽和水蒸気圧曲線に沿うように加温および冷却するように前記ヒーターのオンオフ制御および前記電磁弁の開閉制御をし、前記ヒーターにより前記圧力容器内を加温する際、前記電磁弁を開いて加温を開始すると共に、前記温度センサにより検出される前記圧力容器内温度が該圧力容器内の水が沸騰する温度に到達する前に、前記電磁弁を閉じて、引き続いて前記圧力容器内が前記所要温度になるまで加温するように前記ヒーターおよび前記電磁弁を制御することを特徴とする。
Therefore, this embodiment is designed to solve the above problems, and the purpose of the present embodiment is to avoid boiling water during the pyrolysis treatment and to saturate the temperature and pressure in the pressure vessel. It is an object of the present invention to provide a thermal decomposition treatment apparatus for an object to be treated and a method for thermal decomposition treatment of the object to be processed, which can be controlled to rise and fall along a pressure curve.
In order to achieve the above object, the present embodiment includes the following configurations.
That is, the thermal decomposition treatment apparatus for the object to be processed according to the present embodiment includes a pressure vessel, a lid for opening and closing the pressure vessel, a temperature sensor for detecting the temperature inside the pressure vessel, and the pressure vessel. A pressure sensor that detects pressure, an electromagnetic valve that can open the pressure vessel to the atmosphere, a heater that heats the inside of the pressure vessel, temperature data detected by the temperature sensor, and pressure detected by the pressure sensor. Data is input, and based on the data, the output of the heater is controlled and the electromagnetic valve is opened and closed to raise the temperature inside the pressure vessel to 125 ° C. to 149 ° C. In the thermal decomposition treatment apparatus for the object to be processed, which has a control unit for thermally decomposing the plant raw material contained in the object to be processed , the control unit is used when the heater is turned on to heat the inside of the pressure vessel. When the heater is turned off to cool the inside of the pressure vessel, the on / off control of the heater and the on / off control of the heater so as to heat and cool the water in the pressure vessel without boiling and along the saturated water vapor pressure curve. When the opening and closing of the electromagnetic valve is controlled and the inside of the pressure vessel is heated by the heater, the electromagnetic valve is opened to start heating, and the temperature inside the pressure vessel detected by the temperature sensor is the pressure vessel. The heater and the electromagnetic valve are controlled so as to close the electromagnetic valve and subsequently heat the inside of the pressure vessel to the required temperature before the water in the pressure vessel reaches a boiling temperature. And.
前記制御部は、前記圧力センサにより検出される圧力が、前記温度センサにより検出される温度と、予め入力されている飽和水蒸気圧曲線の近似式とから演算される演算圧力値に近接するように、前記ヒーターの出力を制御すると好適である。 In the control unit, the pressure detected by the pressure sensor is close to the calculated pressure value calculated from the temperature detected by the temperature sensor and the approximate expression of the saturated water vapor pressure curve input in advance. , It is preferable to control the output of the heater.
また、前記制御部は、前記ヒーターをオフし、前記圧力容器内を冷却する際、前記温度センサにより検出される前記圧力容器内温度が該圧力容器内の水が沸騰する温度よりも低い温度にまで達したときに前記電磁弁を開くように制御すると好適である。 Further, when the control unit turns off the heater and cools the inside of the pressure vessel, the temperature inside the pressure vessel detected by the temperature sensor becomes a temperature lower than the temperature at which the water in the pressure vessel boils. It is preferable to control the electromagnetic valve to open when the temperature reaches the limit.
また、本実施の形態に係る被処理物の熱分解処理方法は、圧力容器と、該圧力容器を開閉する蓋体と、前記圧力容器内の温度を検出する温度センサと、前記圧力容器内の圧力を検出する圧力センサと、前記圧力容器を大気に開放可能な電磁弁と、前記圧力容器内を加温するヒーターとを具備する熱分解処理装置を用いる被処理物の熱分解処理方法において、前記圧力容器内に植物原料を被処理物として収容する工程と、前記圧力容器を前記蓋体で密閉する工程と、前記電磁弁を開くと共に、前記ヒーターにより前記圧力容器内を加温する工程と、前記ヒーターによる加温時、前記温度センサにより検出される前記圧力容器内温度が該圧力容器内の水が沸騰する温度に到達する前に、前記電磁弁を閉じる工程と、引き続いて、前記圧力容器内温度が１２５℃〜１４９℃の温度に上昇するまで、前記ヒーターにより前記圧力容器を加温し、前記植物原料を熱分解する工程と、前記ヒーターによる加温を停止し、前記圧力容器内を冷却する工程と、前記圧力容器内を冷却する際、前記温度センサにより検出される前記圧力容器内温度が該圧力容器内の水が沸騰する温度よりも低い温度にまで達したときに前記電磁弁を開いて、前記圧力容器を大気に開放して前記圧力容器を所要温度にまで冷却する工程を具備し、前記加温時および前記冷却時、前記圧力容器内を、飽和水蒸気圧曲線に沿うように加温および冷却することを特徴とする。 Further, the method for thermally decomposing the object to be treated according to the present embodiment includes a pressure vessel, a lid for opening and closing the pressure vessel, a temperature sensor for detecting the temperature inside the pressure vessel, and a pressure vessel. In a thermal decomposition treatment method for an object to be processed, which uses a thermal decomposition treatment apparatus including a pressure sensor for detecting pressure, an electromagnetic valve capable of opening the pressure vessel to the atmosphere, and a heater for heating the inside of the pressure vessel. A step of accommodating a plant material in the pressure vessel as an object to be processed, a step of sealing the pressure vessel with the lid, and a step of opening the electromagnetic valve and heating the inside of the pressure vessel with the heater. During heating by the heater, the step of closing the electromagnetic valve before the temperature inside the pressure vessel detected by the temperature sensor reaches the temperature at which the water in the pressure vessel boils, followed by the pressure. The pressure vessel is heated by the heater until the temperature inside the vessel rises to a temperature of 125 ° C. to 149 ° C., the step of thermally decomposing the plant raw material , and the heating by the heater are stopped, and the inside of the pressure vessel is stopped. And when the inside of the pressure vessel is cooled, the electromagnetic wave is detected when the temperature inside the pressure vessel reaches a temperature lower than the temperature at which the water in the pressure vessel boils. A step of opening a valve, opening the pressure vessel to the atmosphere, and cooling the pressure vessel to a required temperature is provided, and the inside of the pressure vessel is followed by a saturated water vapor pressure curve during heating and cooling. It is characterized by heating and cooling as described above.
前記圧力センサにより検出される圧力が、前記温度センサにより検出される温度と、飽和水蒸気圧曲線の近似式とから演算される演算圧力値に近接するように、前記ヒーターの出力を制御すると好適である。 It is preferable to control the output of the heater so that the pressure detected by the pressure sensor is close to the calculated pressure value calculated from the temperature detected by the temperature sensor and the approximate expression of the saturated water vapor pressure curve. be.
本発明によれば、熱分解処理中に水の沸騰するのを回避し、圧力容器内の温度、圧力を飽和水蒸気圧曲線に沿って上昇、下降するよう制御することのできる被処理物の熱分解処理装置および被処理物の熱分解処理方法を提供できる。 According to the present invention, it is possible to avoid boiling water during the pyrolysis treatment and control the temperature and pressure in the pressure vessel to rise and fall along the saturated water vapor pressure curve. A decomposition processing apparatus and a method for thermally decomposing an object to be processed can be provided.
以下本発明の実施の形態を添付図面を参照して詳細に説明する。
図１Ａは、熱分解処理装置の縦断面図、図１Ｂはその平面図である。
熱分解処理装置は、ハッチを開閉する蓋体１を備えた円筒状の圧力容器２をなす。圧力容器２の下底および外周面にはヒーター３が装着され、圧力容器２内の温度は温度センサ４によって検知される。なお、圧力容器２の底部の温度及び周面の温度は別個に制御される。圧力容器２内の温度検知信号は制御装置（制御部）５に伝送される。
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
FIG. 1A is a vertical sectional view of the thermal decomposition processing apparatus, and FIG. 1B is a plan view thereof.
The pyrolysis treatment device forms a cylindrical pressure vessel 2 provided with a lid 1 for opening and closing the hatch. Heaters 3 are mounted on the lower bottom and the outer peripheral surface of the pressure vessel 2, and the temperature inside the pressure vessel 2 is detected by the temperature sensor 4. The temperature at the bottom of the pressure vessel 2 and the temperature at the peripheral surface are controlled separately. The temperature detection signal in the pressure vessel 2 is transmitted to the control device (control unit) 5.
蓋体１には圧力容器２内の圧力を検出する圧力センサ６と、圧力コントロール用の電磁弁７が取り付けられている。電磁弁７は、制御装置５からの指示によって開弁し、圧力容器２内に発生させた水蒸気を外部に排出して圧力容器２内の圧力をコントロールするものである。
A pressure sensor 6 for detecting the pressure in the pressure vessel 2 and an electromagnetic valve 7 for pressure control are attached to the lid 1. The solenoid valve 7 opens according to an instruction from the
被処理物は、かご８内に収容して圧力容器２内のほぼ中央領域に差し入れられる。また、圧力容器２の底には、被処理物から搾り出された抽出液及び容器の壁面を伝わって落ちる可溶性成分の凝縮液を受け入れるトレー１１を格納しておく。 The object to be processed is housed in the car 8 and inserted into a substantially central region in the pressure vessel 2. Further, in the bottom of the pressure vessel 2, a tray 11 for receiving the extract squeezed from the object to be treated and the condensate of the soluble component that falls down the wall surface of the container is stored.
図２に、圧力容器２内で進行させる水蒸気分解反応の進行を監視するためのシステムの構成を示す。制御装置５は、監視室９内に設置されたコンピューターであり、ヒーターの電源投入（ＯＮ、ＯＦＦ）、処理時間の設定、電磁弁７の開閉制御などの制御を行う。さらに制御装置５は、成分抽出処理に必要な一切の制御並びに設定情報の管理を行う機能、分解反応の進行状況の監視機能を実行し、植物組織から抽出される物質の抽出進行状態は、モニター１０によって監視するほか、これらのデータをオートサンプラ１２に収集してサンプリングを行う機能を有している。
FIG. 2 shows the configuration of a system for monitoring the progress of the steam decomposition reaction that proceeds in the pressure vessel 2. The
制御装置５は、植物原料Ａを洗浄し、必要により適当な大きさに裁断あるいは不要部分を除去した被処理物Ｂを圧力容器２内に収容して成分抽出処理Ｃを施し、成分抽出処理Ｃによって得られた抽出液Ｄを圧力容器２から取り出し、これに精製処理Ｅを施すことによって、高純度の植物組織成分を得るまでの処理を管理する。
The
成分抽出処理（熱分解処理）Ｃに先立って、圧力容器２のハッチを開き、圧力容器２内に少量の水を注入する。
次に成分抽出処理Ｃを施すべき被処理物Ｂをかご８の中に入れ、これを圧力容器２内に格納してハッチを閉じ、圧力容器２内で被処理物Ｂの成分抽出処理Ｃを開始する。処理の手順を図３〜図５に従って説明する。
Prior to the component extraction treatment (pyrolysis treatment) C, the hatch of the pressure vessel 2 is opened, and a small amount of water is injected into the pressure vessel 2.
Next, the object B to be subjected to the component extraction process C is placed in the basket 8, stored in the pressure vessel 2, the hatch is closed, and the component extraction process C of the object B to be processed is performed in the pressure vessel 2. Start. The processing procedure will be described with reference to FIGS. 3 to 5.
図３、図４は、熱分解処理を実行する手順を示すフロー図である。
図３、図４に示すように、まず、内外をつなぐ管路に設けられた電磁弁７を開いて圧力容器２を大気に開放すると共に、ヒーター３の電源を投入（ＯＮ）する（ステップＳ１、ステップＳ２）。
ヒーター３による圧力容器２の加温中、適宜時間間隔をおいて、圧力容器２内の温度（ｔ）、圧力（ｐ）を温度センサ４、圧力センサ６によってそれぞれ検出する（ステップＳ３）。
3 and 4 are flow charts showing a procedure for executing the thermal decomposition treatment.
As shown in FIGS. 3 and 4, first, the solenoid valve 7 provided in the conduit connecting the inside and the outside is opened to open the pressure vessel 2 to the atmosphere, and the heater 3 is turned on (ON) (step S1). , Step S2).
While the pressure vessel 2 is being heated by the heater 3, the temperature (t) and the pressure (p) in the pressure vessel 2 are detected by the temperature sensor 4 and the pressure sensor 6 at appropriate time intervals (step S3).
検出温度データおよび検出圧力データはその都度制御部５に伝送され、制御部５では、検出された温度が、設定温度範囲（例えば７０℃〜８０℃）内であるか否か判定する。
この設定温度範囲は、圧力容器２内の水が沸騰に至らない温度とし、安全のため、７０℃〜８０℃の温度範囲とするのがよい（７０℃〜９０℃程度でもよい）。
The detected temperature data and the detected pressure data are transmitted to the
This set temperature range is set to a temperature at which the water in the pressure vessel 2 does not reach boiling, and for safety, it is preferably set to a temperature range of 70 ° C. to 80 ° C. (may be about 70 ° C. to 90 ° C.).
本実施の形態では、上記のように電磁弁７を開いて、圧力容器２内を大気に開放した状態でヒーター３にて加温する。これにより、水蒸気圧が増すにしたがって、圧力容器２内の空気は排除される。したがって、圧力容器２内の温度が、８０℃程度であれば、圧力容器２内の空気はほとんど排除され、検出される圧力（実測圧力値）は、ほとんど飽和水蒸気圧に近いものとなる。 In the present embodiment, the solenoid valve 7 is opened as described above, and the pressure vessel 2 is heated by the heater 3 in a state of being open to the atmosphere. As a result, the air in the pressure vessel 2 is eliminated as the water vapor pressure increases. Therefore, when the temperature in the pressure vessel 2 is about 80 ° C., the air in the pressure vessel 2 is almost eliminated, and the detected pressure (measured pressure value) is almost close to the saturated water vapor pressure.
検出温度が、温度設定温度範囲に至っていない場合にはステップＳ３および上記判定を繰り返す。
温度計測は、できるだけ狭い温度上昇幅（例えば５℃程度）ごとになるように行うのが、沸騰回避上、安全でよい。
検出温度が上記設定温度に至った場合、電磁弁７を閉じる（ステップＳ４）。ヒーター３による加温は継続する。
If the detected temperature does not reach the temperature set temperature range, step S3 and the above determination are repeated.
It is safe to measure the temperature so that the temperature rises as narrowly as possible (for example, about 5 ° C.) in order to avoid boiling.
When the detected temperature reaches the above set temperature, the solenoid valve 7 is closed (step S4). Heating by the heater 3 continues.
電磁弁７を閉じて後、適宜な段階でタイマー（図示せず）により、熱分解処理時間を例えば３時間にセットする（ステップＳ５）。
また、適宜な時間間隔（あるいは適宜な温度上昇幅ごと）で圧力容器２内の温度（ｔ）と圧力（ｐ）を検出する（ステップＳ６）。
検出温度データ、検出圧力データはその都度制御装置５に伝送され、制御装置５では、予め入力されている飽和水蒸気圧曲線の近似式に、温度センサ４で検出された温度数値を代入して、当該近似式に基づく飽和水蒸気圧（演算圧力値）を演算する（ステップＳ７）。近似式としては、Ｔｅｔｅｎｓの式などを用いることができるが、これに限定されるものではない。
After closing the solenoid valve 7, the thermal decomposition processing time is set to, for example, 3 hours by a timer (not shown) at an appropriate stage (step S5).
Further, the temperature (t) and the pressure (p) in the pressure vessel 2 are detected at appropriate time intervals (or at appropriate temperature rise widths) (step S6).
The detected temperature data and the detected pressure data are transmitted to the
また制御装置５では、この演算圧力値と圧力センサ６で検出される圧力値（実測圧力値）とを比較し、実測圧力値の演算圧力値に対するずれが所要設定範囲内であるか否か判定する（ステップＳ８）。
実測圧力値が演算圧力値に対して設定範囲以上にずれている場合には、ヒーター３の出力を調整し（ステップ９）、実測圧力値が演算圧力値にできるだけ近接するように制御する。
なお、ステップＳ４に至る段階でも、ステップＳ６〜ステップＳ９と同様の制御をし、実測圧力値が演算圧力値に近接するようにヒーター３のＯＮ、ＯＦＦ制御をするようにしてもよい。
Further, the
When the measured pressure value deviates from the calculated pressure value by a set range or more, the output of the heater 3 is adjusted (step 9), and the measured pressure value is controlled so as to be as close as possible to the calculated pressure value.
Even at the stage leading to step S4, the same control as in steps S6 to S9 may be performed, and the heater 3 may be ON / OFF controlled so that the measured pressure value is close to the calculated pressure value.
ステップ６〜ステップ９の制御を行いつつ、ステップＳ６における検出温度が、１２５℃〜１４９℃内の設定温度まで上昇したら（ステップＳ１１）、ヒーター３の出力を調整（あるいはＯＦＦ）して（ステップ１０）、タイマーでセットした時間だけ上記設定温度に維持し、必要な、熱分解処理を行う。 While controlling steps 6 to 9, when the detection temperature in step S6 rises to a set temperature within 125 ° C. to 149 ° C. (step S11), the output of the heater 3 is adjusted (or turned off) (step 10). ), Maintain the above set temperature for the time set by the timer, and perform the necessary thermal decomposition treatment.
なお、本実施形態における熱分解処理は、圧力容器２内温度が１２５℃〜１４９℃の範囲で行うのがよいが、被処理物の種類に応じて、この温度範囲内で設定温度を決定するとよい。温度１５０℃以上に上昇すると、被処理物が炭化してしまう。
タイマーがＯＦＦとなったら（ステップＳ１１）、ヒーターをＯＦＦにする（ステップＳ１２）。
上記のようにすることで、ステップＳ１２に至るまで、圧力容器２内の温度、圧力をほぼ飽和水蒸気圧曲線に沿って上昇するように制御することができる。
The thermal decomposition treatment in the present embodiment is preferably performed in the temperature range of 125 ° C. to 149 ° C. in the pressure vessel 2, but if the set temperature is determined within this temperature range according to the type of the object to be treated. good. If the temperature rises above 150 ° C, the object to be treated will be carbonized.
When the timer is turned off (step S11), the heater is turned off (step S12).
By doing so, it is possible to control the temperature and pressure in the pressure vessel 2 so as to rise substantially along the saturated water vapor pressure curve until step S12.
本実施の形態では、ヒーター３をＯＦＦしたまま、圧力容器２を自然冷却する（ステップＳ１３）。
この自然冷却することによって、圧力容器２内は、温度、圧力がほぼ飽和水蒸気圧曲線に沿ったまま降下することになる。
この間、適宜時間間隔ごとに温度センサ４により圧力容器２内の温度を検出する（ステップＳ１４）。検出温度が、例えば、９０℃程度の、水の沸騰を回避できる程度の温度にまで降下したら、電磁弁７を開き（ステップＳ１５）、このまま圧力容器２内を自然冷却して（ステップＳ１６）処理を終了する。
In the present embodiment, the pressure vessel 2 is naturally cooled while the heater 3 is turned off (step S13).
By this natural cooling, the temperature and pressure inside the pressure vessel 2 will drop while substantially following the saturated water vapor pressure curve.
During this time, the temperature inside the pressure vessel 2 is detected by the temperature sensor 4 at appropriate time intervals (step S14). When the detection temperature drops to, for example, about 90 ° C., a temperature at which boiling of water can be avoided, the solenoid valve 7 is opened (step S15), and the inside of the pressure vessel 2 is naturally cooled as it is (step S16). To finish.
このようにして、ステップＳ１２以降も、圧力容器２内の温度、圧力をほぼ飽和水蒸気圧曲線に沿って下降するように制御することができる。ステップＳ１５に示すように、圧力容器２内温度が９０℃以下に低下した際に電磁弁７を開くようにしているので、圧力容器２内の水の沸騰を確実に防止できる。 In this way, even after step S12, the temperature and pressure in the pressure vessel 2 can be controlled so as to decrease substantially along the saturated water vapor pressure curve. As shown in step S15, since the solenoid valve 7 is opened when the temperature inside the pressure vessel 2 drops to 90 ° C. or lower, boiling of water in the pressure vessel 2 can be reliably prevented.
なお、圧力容器２が大型で、ステップＳ１３における自然冷却するのに長時間を要する場合には、ステップＳ１２でヒーターをＯＦＦした後、電磁弁７を所定時間間隔ごとに短時間開いて水蒸気を逃がすことにより、圧力容器２内の冷却速度を大きくして冷却するようにしてもよい。 If the pressure vessel 2 is large and it takes a long time to cool naturally in step S13, after turning off the heater in step S12, the electromagnetic valve 7 is opened for a short time at predetermined time intervals to release water vapor. As a result, the cooling rate inside the pressure vessel 2 may be increased for cooling.
この場合、圧力容器２内の温度と圧力をそれぞれ温度センサ４、圧力センサ６で検出し、上記と同様にして、飽和水蒸気圧曲線の近似式により、検出温度における演算圧力を算出し、実測圧力が演算圧力に近接するように、電磁弁７の開放間隔、開放時間を制御するようにするとよい。これにより、冷却時においても、圧力容器２内の水を沸騰させることなく、圧力容器２内の温度、圧力を飽和水蒸気圧曲線に沿って降下させるように制御できる。 In this case, the temperature and pressure in the pressure vessel 2 are detected by the temperature sensor 4 and the pressure sensor 6, respectively, and the calculated pressure at the detected temperature is calculated by the approximate expression of the saturated water vapor pressure curve in the same manner as described above, and the measured pressure is measured. It is preferable to control the opening interval and opening time of the electromagnetic valve 7 so that the pressure is close to the calculated pressure. Thereby, even at the time of cooling, the temperature and pressure in the pressure vessel 2 can be controlled to be lowered along the saturated water vapor pressure curve without boiling the water in the pressure vessel 2.
図１、図２に示す熱分解処理装置を用いて、図３、図４に示す処理手順により、柿実および柿皮の少なくとも一方の柿材料の熱分解処理を行った。
本実施例においては、柿実および柿皮の少なくとも一方の柿材料を圧力容器２内に収容する工程と、該圧力容器２内に必要量の水を供給し、圧力容器２内をヒーター３により２時間〜５時間の間加熱して、柿材料の細胞や細胞壁が破壊すると共に、酵素の作用によりタンニンの生成を促進し、柿材料中に含まれるタンニン量が、生柿のタンニン量よりも多くなるようにする加熱工程と、圧力容器２内を冷却する冷却工程と、冷却後圧力容器２内から産出物を回収する回収工程とを行い、柿加工品を得た。
Using the thermal decomposition treatment apparatus shown in FIGS. 1 and 2, at least one of the persimmon material of the persimmon fruit and the persimmon skin was thermally decomposed by the treatment procedure shown in FIGS. 3 and 4.
In this embodiment, a step of accommodating at least one persimmon material of persimmon fruit and persimmon skin in the pressure vessel 2 and supplying a required amount of water into the pressure vessel 2 and using a heater 3 in the pressure vessel 2 Heating for 2 to 5 hours destroys the cells and cell walls of the persimmon material and promotes the production of tannin by the action of enzymes, and the amount of tannin contained in the persimmon material is larger than the amount of tannin in raw persimmon. A persimmon processed product was obtained by performing a heating step for increasing the number of persimmons, a cooling step for cooling the inside of the pressure vessel 2, and a recovery step for recovering the product from the pressure vessel 2 after cooling.
圧力容器２内の加熱、および冷却は、上記手順にしたがって、温度、圧力が飽和水蒸気圧曲線に沿って上昇、下降するように制御した。
その結果、後記するように、生柿におけるタンニン量は、タンニン酸として、１００ｇ中、約０．１３ｇであるが、得られた柿加工品のタンニン含有量は、タンニン酸として、１００ｇ中、約０．３７ｇ〜約０．６３ｇとなり、生柿の約３〜５倍に増量していた。
The heating and cooling in the pressure vessel 2 were controlled so that the temperature and pressure increased and decreased along the saturated water vapor pressure curve according to the above procedure.
As a result, as will be described later, the amount of tannin in the raw persimmon is about 0.13 g in 100 g of tannic acid, but the tannin content of the obtained processed persimmon product is about 0.13 g in 100 g of tannic acid. The amount was 0.37 g to about 0.63 g, which was about 3 to 5 times as much as that of raw persimmon.
なお、上記水蒸気熱分解処理を行う場合、圧力容器２内を１２０℃〜１３４℃（１３４℃以下）の温度で加熱するとさらに好適である。タンニン生成を促進する酵素は、１３４℃位までその酵素活性が維持あるいは向上し、１３５℃以上になるとその酵素活性が次第に低下するからである。例えば、後記するように、柿皮を１３２℃で４時間水蒸気分解処理をして得られたエキス中のタンニン量は、タンニン酸として、１００ｇ中、約０．４８ｇであったが、柿皮を１３７℃で４時間水蒸気分解処理をして得られたエキス中のタンニン量は、タンニン酸として、１００ｇ中、約０．３７ｇとなって、１３２℃での処理の場合よりも少なくなっている。 When the steam pyrolysis treatment is performed, it is more preferable to heat the inside of the pressure vessel 2 at a temperature of 120 ° C. to 134 ° C. (134 ° C. or lower). This is because the enzyme activity that promotes tannin production is maintained or improved up to about 134 ° C., and the enzyme activity gradually decreases at 135 ° C. or higher. For example, as described later, the amount of tannin in the extract obtained by subjecting the persimmon bark to steam decomposition treatment at 132 ° C. for 4 hours was about 0.48 g in 100 g of tannic acid, but the persimmon bark was used. The amount of tannin in the extract obtained by steam decomposition treatment at 137 ° C. for 4 hours was about 0.37 g in 100 g of tannic acid, which was less than that in the case of treatment at 132 ° C.
産出物の回収に際しては、図示しないドレインバルブを開いて圧力容器２内部に冷却コイルより冷却水を送り込み、圧力容器２内の水蒸気を冷却して結露させることによって生じた蒸留液（エキス）をドレインタンクに回収する。
次いで、圧力容器２の蓋体を開き、水蒸気熱分解処理によって圧力容器２内のトレー１１に生成された溶出液（エキス）を回収し、さらに、処理物かご８を圧力容器２内から搬出して、処理物かご８から固形物を回収する。固形物は、乾燥して粉末化するとよい。
When recovering the product, the drain valve (not shown) is opened, cooling water is sent from the cooling coil into the pressure vessel 2, and the water vapor in the pressure vessel 2 is cooled to cause dew condensation, thereby draining the distilled liquid (extract). Collect in a tank.
Next, the lid of the pressure vessel 2 is opened, the eluate (extract) generated in the tray 11 in the pressure vessel 2 by the steam pyrolysis treatment is collected, and the processed product basket 8 is further carried out from the pressure vessel 2. Then, the solid matter is collected from the processed product basket 8. The solid material may be dried and pulverized.
[具体的実施例１]
冷凍保存された喬木村産の市田柿（登録商標）の実および皮を水蒸気分解処 理をし、そのエキスおよび固形分と、冷凍保存された原料柿（生柿）とに含ま れるタンニン酸をイオン交換法により分析した（分析試験は、一般財団法人日 本食品分析センターに依頼）。
<サンプル製造方法>
柿実および柿皮を、図１に示す熱分解処理装置を用いて１３２℃、約３．０ 気圧の飽和水蒸気中に４．０時間曝したサンプル（エキスおよび固形分）と、 同１３７℃、約３．３気圧の飽和水蒸気中に４．０時間曝したサンプル（エキ スおよび固形分）を作成した。
<タンニン酸分析試験>
冷凍保存された原料柿（皮）および上記サンプル中のタンニン酸含量の分析試験結果（一般財団法人日本食品分析センター）を表１に示す。
[Specific Example 1]
Tannic acid contained in the frozen and preserved raw persimmon (raw persimmon) of Ichida persimmon (registered trademark) from Takagi village, which is processed by steam decomposition and its extract and solid content. Was analyzed by the ion exchange method (the analysis test was requested to the Japan Food Research Laboratories).
<Sample manufacturing method>
A sample (extract and solid content) of persimmon seeds and persimmon bark exposed to saturated steam at 132 ° C. and about 3.0 atm for 4.0 hours using the pyrolysis treatment device shown in FIG. 1 and a sample (extract and solid content) at 137 ° C. Samples (extracts and solids) exposed to saturated water vapor at about 3.3 atm for 4.0 hours were prepared.
<Tannic acid analysis test>
Table 1 shows the results of the analysis test of the tannic acid content in the frozen raw persimmon (skin) and the above sample (Japan Food Research Laboratories).
また、１３２℃での水蒸気分解処理サンプルの方が、１３７℃での水蒸気分解処理サンプルよりもタンニン量が増えている。
また、柿皮エキスＡ、Ｂの場合に比して、柿実エキスＢおよび柿実皮混合エキスＡにおけるタンニン量がその約１．５倍と多いことから、柿実の方が、柿皮よりもタンニン量が多いことがわかった。
なお、タンニン量は、柿の種類によっても相違すると考えられる。
In addition, the amount of tannin in the steam-decomposed sample at 132 ° C. is larger than that in the steam-decomposition-treated sample at 137 ° C.
In addition, since the amount of tannin in the persimmon fruit extract B and the persimmon skin mixed extract A is about 1.5 times larger than that in the case of the persimmon skin extracts A and B, the persimmon fruit is more than the persimmon skin. It was found that the amount of tannin was also large.
The amount of tannin is considered to differ depending on the type of persimmon.
柿皮エキスＢ（１３２℃水蒸気分解処理）のエネルギー分を測定したところ、約４７ｋｃａｌ／１００ｇであって、砂糖の約１／１０となり、低カロリーである。
また、各サンプルを食したところ、渋みはほとんど感じられなかった。水蒸気分解処理を行ったことにより、タンニンが低分子化し、渋みが低減したと考えられる。また、柿本来の甘さが感じられ、実際柿皮エキスＢの糖度を糖度計で測定したところ約１８°の糖度となり、低カロリーの砂糖代替甘味料として十分使用できることがわかった。
また、実際に柿皮エキスＢを湯に溶いて飲用したところ、香ばしく、まろやかでコーヒー様の味がし、そのままでも飲食品として十分に適していることがわかった。
なお、本実施例で得られた柿加工品は、甘味料以外の食品添加材として用いることができるほか、タンニンを含むことから各種抗菌剤等としても用いることができる。
When the energy content of persimmon bark extract B (steam decomposition treatment at 132 ° C.) was measured, it was about 47 kcal / 100 g, which was about 1/10 of that of sugar, and was low in calories.
Moreover, when each sample was eaten, almost no astringency was felt. It is considered that the water vapor decomposition treatment reduced the molecular weight of tannins and reduced astringency. In addition, the original sweetness of the persimmon was felt, and when the sugar content of the persimmon skin extract B was actually measured with a sugar content meter, the sugar content was about 18 °, and it was found that it could be sufficiently used as a low-calorie sugar substitute sweetener.
Moreover, when the persimmon skin extract B was actually dissolved in hot water and drunk, it was found that it had a fragrant, mellow and coffee-like taste, and was sufficiently suitable as a food and drink as it was.
The processed persimmon product obtained in this example can be used as a food additive other than a sweetener, and can also be used as various antibacterial agents because it contains tannin.
１ 蓋体、２ 圧力容器、３ ヒーター、４ 温度センサ、５ 制御装置（制御部）、６ 圧力センサ、７ 電磁弁、８ かご、１０ モニター、１１ トレー、１２ オートサンプラ 1 lid, 2 pressure vessel, 3 heater, 4 temperature sensor, 5 control device (control unit), 6 pressure sensor, 7 solenoid valve, 8 basket, 10 monitor, 11 tray, 12 auto sampler
Claims (5)
前記制御部は、
前記ヒーターをオンして前記圧力容器内を加温する際、および前記ヒーターをオフして前記圧力容器内を冷却する際、前記圧力容器内の水を沸騰させることなく、かつ飽和水蒸気圧曲線に沿うように加温および冷却するように前記ヒーターのオンオフ制御および前記電磁弁の開閉制御をし、
前記ヒーターにより前記圧力容器内を加温する際、前記電磁弁を開いて加温を開始すると共に、前記温度センサにより検出される前記圧力容器内温度が該圧力容器内の水が沸騰する温度に到達する前に、前記電磁弁を閉じて、引き続いて前記圧力容器内が前記所要温度になるまで加温するように前記ヒーターおよび前記電磁弁を制御すること
を特徴とする被処理物の熱分解処理装置。 A pressure vessel, a lid for opening and closing the pressure vessel, a temperature sensor for detecting the temperature inside the pressure vessel, a pressure sensor for detecting the pressure inside the pressure vessel, and an electromagnetic wave capable of opening the pressure vessel to the atmosphere. A valve, a heater that heats the inside of the pressure vessel, temperature data detected by the temperature sensor, and pressure data detected by the pressure sensor are input, and the output of the heater is controlled based on the data. At the same time, it has a control unit that controls the opening and closing of the electromagnetic valve to raise the temperature inside the pressure vessel to 125 ° C. to 149 ° C. and thermally decomposes the plant raw material contained in the pressure vessel as an object to be treated. In the thermal decomposition treatment equipment of the object to be processed
The control unit
When the heater is turned on to heat the inside of the pressure vessel, and when the heater is turned off to cool the inside of the pressure vessel, the water in the pressure vessel is not boiled and the saturated water vapor pressure curve is obtained. On / off control of the heater and opening / closing control of the electromagnetic valve are performed so as to heat and cool along the line.
When the inside of the pressure vessel is heated by the heater, the electromagnetic valve is opened to start heating, and the temperature inside the pressure vessel detected by the temperature sensor becomes the temperature at which the water in the pressure vessel boils. before reaching, by closing the electromagnetic valve, of the object it characterized in that subsequently the pressure vessel to control the heater and the solenoid valve to warm until the required temperature heat Disassembly processing equipment.
前記圧力センサにより検出される圧力が、前記温度センサにより検出される温度と、予め入力されている飽和水蒸気圧曲線の近似式とから演算される演算圧力値に近接するように、前記ヒーターの出力を制御すること
を特徴とする請求項１記載の被処理物の熱分解処理装置。 The control unit
The output of the heater so that the pressure detected by the pressure sensor is close to the calculated pressure value calculated from the temperature detected by the temperature sensor and the approximate expression of the saturated water vapor pressure curve input in advance. The thermal decomposition treatment apparatus for an object to be processed according to claim 1, wherein the device is used for controlling the temperature of the object to be processed.
前記ヒーターをオフし、前記圧力容器内を冷却する際、前記温度センサにより検出される前記圧力容器内温度が該圧力容器内の水が沸騰する温度よりも低い温度にまで達したときに前記電磁弁を開くように制御すること
を特徴とする請求項１または２記載の被処理物の熱分解処理装置。 The control unit
When the heater is turned off and the inside of the pressure vessel is cooled, the electromagnetic wave is detected when the temperature inside the pressure vessel reaches a temperature lower than the temperature at which the water in the pressure vessel boils. The thermal decomposition treatment apparatus for an object to be treated according to claim 1 or 2, wherein the valve is controlled to open.
前記圧力容器内に植物原料を被処理物として収容する工程と、
前記圧力容器を前記蓋体で密閉する工程と、
前記電磁弁を開くと共に、前記ヒーターにより前記圧力容器内を加温する工程と、
前記ヒーターによる加温時、前記温度センサにより検出される前記圧力容器内温度が該圧力容器内の水が沸騰する温度に到達する前に、前記電磁弁を閉じる工程と、
引き続いて、前記圧力容器内温度が１２５℃〜１４９℃の温度に上昇するまで、前記ヒーターにより前記圧力容器を加温し、前記植物原料を熱分解する工程と、
前記ヒーターによる加温を停止し、前記圧力容器内を冷却する工程と、
前記圧力容器内を冷却する際、前記温度センサにより検出される前記圧力容器内温度が該圧力容器内の水が沸騰する温度よりも低い温度にまで達したときに前記電磁弁を開いて、前記圧力容器を大気に開放して前記圧力容器を所要温度にまで冷却する工程を具備し、
前記加温時および前記冷却時、前記圧力容器内を、飽和水蒸気圧曲線に沿うように加温および冷却すること
を特徴とする被処理物の熱分解処理方法。 A pressure vessel, a lid for opening and closing the pressure vessel, a temperature sensor for detecting the temperature inside the pressure vessel, a pressure sensor for detecting the pressure inside the pressure vessel, and an electromagnetic wave capable of opening the pressure vessel to the atmosphere. In a method for thermally decomposing an object to be processed using a thermal decomposition treatment apparatus including a valve and a heater for heating the inside of the pressure vessel.
The step of accommodating the plant raw material as an object to be processed in the pressure vessel, and
The step of sealing the pressure vessel with the lid body and
A step of opening the solenoid valve and heating the inside of the pressure vessel with the heater,
During heating by the heater, the step of closing the electromagnetic valve before the temperature inside the pressure vessel detected by the temperature sensor reaches the temperature at which the water in the pressure vessel boils.
Subsequently, a step of heating the pressure vessel with the heater and thermally decomposing the plant raw material until the temperature inside the pressure vessel rises to a temperature of 125 ° C. to 149 ° C.
The step of stopping the heating by the heater and cooling the inside of the pressure vessel,
When cooling the inside of the pressure vessel, the electromagnetic valve is opened when the temperature inside the pressure vessel detected by the temperature sensor reaches a temperature lower than the temperature at which the water in the pressure vessel boils. A step of opening the pressure vessel to the atmosphere and cooling the pressure vessel to a required temperature is provided.
A method for thermally decomposing an object to be treated, which comprises heating and cooling the inside of the pressure vessel at the time of heating and cooling so as to follow a saturated water vapor pressure curve.
を特徴とする請求項４記載の被処理物の熱分解処理方法。 Controlling the output of the heater so that the pressure detected by the pressure sensor is close to the calculated pressure value calculated from the temperature detected by the temperature sensor and the approximate expression of the saturated water vapor pressure curve. The method for thermally decomposing an object to be treated according to claim 4.
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