JP4636664B2 - High-temperature and high-pressure vessel with microwave supply device for chemical reaction promotion - Google Patents

High-temperature and high-pressure vessel with microwave supply device for chemical reaction promotion Download PDF

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JP4636664B2
JP4636664B2 JP2000311198A JP2000311198A JP4636664B2 JP 4636664 B2 JP4636664 B2 JP 4636664B2 JP 2000311198 A JP2000311198 A JP 2000311198A JP 2000311198 A JP2000311198 A JP 2000311198A JP 4636664 B2 JP4636664 B2 JP 4636664B2
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pressure
temperature
vessel
reaction
window
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JP2002113350A (en
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俊作 加藤
眞昊 李
栄 堀川
博文 曽我
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Shikoku Instrumentation Co Ltd
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Shikoku Instrumentation Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
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Description

【0001】
【産業上の利用分野】
本発明は、化学反応の促進または収率の向上を可能にする、化学反応促進用マイクロ波供給装置を設けた高温高圧容器に関する。
【0002】
【従来の技術】
マイクロ波を利用した化学反応は試みられ始めて15年程度と年月が浅く、系統的な化学の基礎が整っておらず、工業技術への展開のための基礎的設計概念を与えるような体系は存在しない。しかしながら、マイクロ波による著しい反応速度(または収率)の向上や従来の加熱法とは異なる反応が促進するなどマイクロ波による化学反応促進効果が認められている(特開平11−21127)。これらの効果はしばしばマイクロ波による加熱効果以外の効果または加熱効果以上の効果という観点からマイクロ波効果またはマイクロ波電界効果或いは非熱的効果と呼ばれている。また、非熱的効果に加え局所加熱反応促進効果および局所反応場の形成による反応促進効果なども示唆されている。
【0003】
一般に高温高圧下での処理物を処理することにより化学反応は促進される。そのための加熱源としては電気ヒーター、バーナー、蒸気などが使用されるが、それらは何れも被加熱物を外部からまたは表面から加熱する手法である(外部加熱法)。現在稼働している化学プラントもその多くは外部加熱法を用いている。本装置は現在稼働しているプラントを改造しマイクロ波を導入し、マイクロ波加熱を利用することにより、又外部加熱とマイクロ波加熱の併用により反応プロセス、収率、反応時間を改善し化学反応を促進させ省エネルギー型プロセスを可能とする。
【0004】
高温高圧条件下でのマイクロ波による加熱装置としては、特開平4−272688、特開平5−251175、特開平5−251176、実開平5−72092が有るが、何れもマイクロ波は単なる加熱源として使用しているにすぎず、また、マイクロ波の供給方法も高温高圧容器の壁部分に窓またはブロックを取付けマイクロ波を供給するものである。
【0005】
【発明が解決しようとする課題】
上記のように従来の方法または装置では、窓またはブロックは、耐熱、耐圧、耐腐食の特性を一度に有する材料および構造が必要であり、また、従来の装置では高温高圧容器内の任意の位置にマイクロ波を供給することができないという問題があった。
そこで、本発明は、上記従来の装置の有する問題点を解決することを課題とする。より具体的には本発明は、窓の制限を緩和した化学反応促進用マイクロ波供給装置を設けた高温高圧容器を提供することを目的とする。
また本発明は、局所的に高温高圧状態を形成させることができ、そのような局所反応場形成により反応を促進させることができる化学反応促進用マイクロ波供給装置を設けた高温高圧容器を提供することを目的とする。
【0006】
【課題を解決するための手段】
本発明は、貫通口を有する耐圧容器と、耐圧容器の内側に設置された耐熱および耐食性の密閉式反応容器とを備え、先端第1の窓を設置した中空の導波管または同軸線路を有する化学反応促進用マイクロ波供給装置の前記先端部を前記貫通口に挿入して耐圧容器内に位置するように設けて導波管または同軸線路を介して被加熱物にマイクロ波を照射するための高温高圧容器であって耐圧容器と反応容器の内圧を等しくするための制御手段を設けたことを特徴とする高温高圧容器を要旨としている。
【0007】
上記の反応容器が、マイクロ波透過性物質で構成された密閉式反応容器であことを特徴とする高温高圧容器を要旨としている
【0008】
また本発明は、上記の耐圧容器の外側に位置する導波管または同軸線路の途中に設置した第2の窓を備えることを特徴とする高温高圧容器を要旨としている。
【0009】
また本発明は、上記の耐圧容器内に取付けた圧力センサーを上記の第1の窓と第2の窓の間にも取付け、第1の窓と第2の窓の間の内圧を制御できるようにした、好ましくは高温高圧条件での反応時に第1の窓と第2の窓の間の内圧を耐圧容器の内圧と等しくなるように制御したことを特徴としている。
【0010】
また本発明は、上記の導波管または同軸線路複数本を耐圧容器中に導入し、反応容器中の大容量の被加熱物を均一に、かつ、広い範囲に加熱できるようにしていることを特徴としている。
【0011】
また本発明は、上記の耐圧容器としての管路中に上記の導波管または同軸線路の複数本を流れに沿って配置し、反応容器中を流通する被加熱物を連続的に加熱できるようにしたことを特徴としている。
【0012】
また本発明は、上記の容器中の被加熱物は、マイクロ波吸収体および/またはマイクロ波吸収性触媒を存在させた高温高圧反応系、亜・超臨界状態にある高温高圧流体系、および/または、電解反応系・光化学反応系・超音波を用いた反応系・外部加熱法を用いた反応系であることを特徴としている。
【0013】
温度センサーおよび圧力センサーを容器内に取付け、それらセンサーの検出値にもとづきマイクロ波出力を制御して容器内の圧力および温度を設定値に保持できるようにしたことを特徴としている。
【0014】
容器に観測用窓を取付け、目視、ファイバースコープによる観測およびリアルタイムでの分光計測を可能にしたことを特徴としている。
【0015】
【実施の形態】
本発明の耐圧容器および反応容器で構成される高温高圧容器への化学反応促進用マイクロ波供給装置は、次の構成を備えることを特徴とする。
中空の導波管または同軸線路を高温高圧容器を構成する耐圧容器中に導入し、その開口部が反応容器中の被加熱物の任意の位置を効率的にマイクロ波により加熱できるようにすること。
複数の導波管または同軸線路を耐圧容器中に導入し、反応容器中の大容量の被加熱物を均一に又広い範囲に加熱できるようにすること。
管路中に複数の導波管または同軸線路を流れに沿って配置し、反応容器中に流通する被加熱物を連続的に加熱できるようにすること。
超臨界状態へマイクロ波により加熱し化学反応を促進できるようにすること。
加熱手段にマイクロ波加熱と外部加熱とを併用すること。
温度センサーを反応容器内に取付け、および圧力センサーを耐圧容器内に取付け、それらセンサーの検出値にもとづきマイクロ波出力を制御して高温高圧容器内の圧力および温度を設定値に保持できるようにすること。
耐圧容器に観測用窓を取付け、目視およびリアルタイムでの分光計測が可能にすること。
【0016】
(1)高温高圧容器は耐圧容器および反応容器で構成され、耐圧容器の内側に耐熱および耐食性の密閉式反応容器を備え、耐圧容器と反応容器の内圧を等しくしたものである。したがって、導波管または同軸線路の第2の窓は基本的には必要がない。
(2)導波管または同軸線路は、開口部に仕切窓としての第1の窓を設置したものであり、好ましくは2つの仕切窓により密閉されている。第1の窓は導波管または同軸線路開口部(マイクロ波照射部、耐圧容器内)に、第2の窓は容器の外側に夫々設置されている。
(3)反応容器はマイクロ波透過性物質(例:石英やテトラフルオロエチレン等)で構成された密閉式反応容器である。
(4)連続式の場合、金属製耐圧容器内にマイクロ波透過性物質で構成された密閉式反応容器がある。反応容器内圧と耐圧容器内圧を等しくなるように制御する。
(5)反応容器は主に耐熱・耐食性であり、第1の窓は主に耐熱・耐圧性(第2の窓がある場合は耐熱性のみ)であり第2の窓は主に耐圧性であり、これらを使い分け制限を緩和する。
(6)高温高圧条件の反応では、容器の圧力(耐圧容器と反応容器の内圧)と第1の窓と第2の窓の間の圧力が等しくなるように第1の窓と第2の窓の間の圧力を制御する。
これにより第1の窓の前後の圧力は等しいため、第1の窓の構造としては主に耐熱・耐腐食という観点からのみその構造を考慮すれば良く薄いシート構造を適用することが可能となる。
また、第2の窓は耐圧容器の外側に設置されるため第2の窓の構造としては主に耐圧という観点からのみその構造を選択すれば良い。
この様に第1の窓と第2の窓の構造を使い分けることにより、高温高圧容器に対する窓の制限を緩和することができる。
【0017】
(7)上記手法によりマイクロ波の浸透深さを考慮し、適当な周波数を選択することにより開口部近傍のみを局所的に加熱することが可能となる。
(8)また加熱したい部分が2箇所以上有る場合は、上記導波管または同軸線路を複数本耐圧容器中に導入することにより、マイクロ波透過性物質で構成された反応容器中の大容量の被加熱物に対しても均一に又広い範囲を加熱することができる。
(8)連続式(流通式)反応の場合には上記導波管または同軸線路を複数本間隔を空けて耐圧容器に取り付けることにより、反応容器中を流通する被加熱物を連続的に加熱することができる。
(9)付加的に冷却、溶液導入などの工程を取り入れることができる。
(10)温度をモニターしマイクロ波出力を制御することにより被加熱物の温度むらを小さくすることができる。
【0018】
【作用】
上記のように構成した化学反応促進用マイクロ波供給装置を有する本発明の高温高圧容器は、第1の窓は耐熱性と耐腐食性を考慮すれば良く、強度は考慮しなくても良いので薄いシート状の構造が採用でき、高温高圧の高温高圧容器に対する窓の制限を緩和することができる。
【0019】
さらに本発明の化学反応促進用マイクロ波供給装置を有する高温高圧容器は、次の作用・効果を奏するものである。被加熱物の任意の位置を効率的にマイクロ波により加熱することができる。大容量の被加熱物を均一に又広い範囲加熱することができる。管路中を流通する被加熱物を連続的に加熱することができる。亜・超臨界状態にある高温・高圧流体系にマイクロ波を導入し化学反応を促進させることができる。反応プロセス、収率、反応時間の改善を図ることができる。反応温度を一定に保つことができ、また、反応状況を目視またはリアルタイムで監視することができる。
高温高圧反応系にマイクロ波吸収体および/またはマイクロ波吸収性触媒を存在させることにより、局所的に高温高圧状態を形成させることができる。そのような局所反応場の形成により反応を促進させることができる。
【0020】
【実施例】
本発明の詳細を実施例で説明する。本発明はこれらの実施例によって何ら限定されるものではない。
【0021】
実施例1
図1は、本発明の第1実施例を示し、耐圧容器および反応容器で構成される高温高圧容器の耐圧容器の天板を貫通して該容器内に先端部が位置するように設けた導波管または同軸線路の挿入端に第1の窓(窓1)を設け、耐圧容器と反応容器の内圧を等しくし、マイクロ波発信器により発振したマイクロ波を導波管または同軸線路を介してマイクロ波透過性物質(石英)でできている反応容器内の被加熱物に照射するように構成してある。
本例では、第2の窓がないので、第1の窓の構造としては主に耐熱・耐圧という観点からその構造を選択することができる。
【0022】
実施例2
図2は、本発明の第2実施例を示し、耐圧容器および反応容器で構成される高温高圧容器の耐圧容器の天板を貫通して該容器内に先端部が位置するように設けた導波管または同軸線路の挿入端に第1の窓(窓1)を設け、導波管または同軸線路の他方の途中に第2の窓(窓2)を設け、耐圧容器内と導波管内を等圧にし、マイクロ波発信器により発振したマイクロ波を導波管または同軸線路を介してマイクロ波透過性物質(石英)でできている反応容器内の被加熱物に照射するように構成してある。
したがって、高温高圧条件の反応では、耐圧容器の圧力と第1の窓と第2の窓の間の圧力が等しくなるように第1の窓と第2の窓の間の圧力を制御すると、第1の窓の前後の圧力は等しくなるので、第1の窓の構造としては主に耐熱・耐腐食という観点からのみその構造を考慮すれば良く薄いシート構造を適用することが可能となり、また、第2の窓は高温高圧の耐圧容器の外側に設置されるため第2の窓の構造としては主に耐圧という観点からのみその構造を選択することができる。
【0023】
上記の導波管または同軸線路は、耐圧容器の天板に摺動可能に装着することができる。その場合、中空の導波管または同軸線路が耐圧容器中に導入され、その開口部が反応容器中の被加熱物(液体またはスラリー)に近接し、被加熱物の任意の位置を効率的にマイクロ波により加熱することができ、また、触媒反応において触媒部のみを選択的に加熱することができる。
開口部が反応容器中の被加熱物に近接し、マイクロ波の浸透深さを考慮し、適当な周波数を選択することにより開口部近傍のみを局所的に加熱することが可能となる。
【0024】
実施例3
図3および図4は、本発明の第3実施例を示し、反応容器に相当する管路を耐圧容器に相当する管路内に同心状に配置した高温高圧容器であって、耐圧容器に相当する管路中に侵入するように複数の導波管または同軸線路を流れに沿って配置し、複数本の導波管または同軸線路の挿入端に第1の窓を設け、導波管または同軸線路の途中に第2の窓を設け、耐圧容器内と導波管内(第1の窓、第2の窓内)を等圧にし、マイクロ波発信器により発振したマイクロ波を導波管または同軸線路を介してマイクロ波透過性物質でできている反応容器内の被加熱物に照射するように構成してある。
したがって、反応容器に相当する管路中を流通する液体を連続的に加熱することができ、さらに、付加的に冷却装置や溶液導入などの工程を取り入れることができ、流路中に温度計Tを配置して温度をモニターしマイクロ波出力を制御することにより被加熱物の温度を設定値に保持することができる。
【0025】
【発明の効果】
本発明により、高温高圧容器における窓の制限を緩和した化学反応促進用マイクロ波供給装置を有する高温高圧容器を提供することができる。また、局所的に高温高圧状態を形成させることができ、そのような局所反応場形成により反応を促進させることができる化学反応促進用マイクロ波供給装置を有する高温高圧容器を提供することができる。
【図面の簡単な説明】
【図1】本発明の化学反応促進用マイクロ波供給装置を有する高温高圧容器の第1実施例の概念図である。
【図2】本発明の化学反応促進用マイクロ波供給装置を有する高温高圧容器の第2実施例の概念図である。
【図3】本発明の化学反応促進用マイクロ波供給装置を有する高温高圧容器の第3実施例の概念図である。
【図4】本発明の化学反応促進用マイクロ波供給装置を有する高温高圧容器の第3実施例の概念図である。
【符号の説明】
G 圧力計
P 加圧ポンプ
T 温度計
V 圧力調整バルブ
[0001]
[Industrial application fields]
The present invention relates to a high-temperature and high-pressure vessel provided with a chemical reaction-promoting microwave supply device that makes it possible to promote chemical reaction or improve yield.
[0002]
[Prior art]
Chemical reactions using microwaves have been attempted for about 15 years, and there is no systematic chemistry foundation, and there is a system that gives basic design concepts for industrial technology development. not exist. However, a chemical reaction promoting effect by microwaves has been recognized, such as a remarkable improvement in reaction rate (or yield) by microwaves and a promotion of reactions different from conventional heating methods (JP-A-11-21127). These effects are often referred to as a microwave effect, a microwave electric field effect, or a non-thermal effect from the viewpoint of an effect other than the heating effect by microwaves or an effect higher than the heating effect. In addition to the non-thermal effect, a local heating reaction promoting effect and a reaction promoting effect by forming a local reaction field are also suggested.
[0003]
In general, a chemical reaction is accelerated by treating an object to be treated under high temperature and pressure. As a heating source for that purpose, an electric heater, a burner, steam, or the like is used, and all of them are methods for heating an object to be heated from the outside or from the surface (external heating method). Many of the chemical plants currently in operation use the external heating method. This equipment improves the reaction process, yield and reaction time by remodeling the currently operating plant, introducing microwaves, using microwave heating, and combining external heating and microwave heating to improve the chemical reaction To promote energy-saving processes.
[0004]
As a heating apparatus using microwaves under high temperature and high pressure conditions, there are JP-A-4-272688, JP-A-5-251175, JP-A-5-251176, and JP-A-5-72092. In addition, the microwave is supplied by attaching a window or a block to the wall portion of the high-temperature and high-pressure vessel and supplying the microwave.
[0005]
[Problems to be solved by the invention]
As described above, in the conventional method or apparatus, the window or block requires a material and a structure having heat resistance, pressure resistance, and corrosion resistance at a time, and in the conventional apparatus, any position in the high-temperature and high-pressure vessel is required. There was a problem that microwaves could not be supplied.
Therefore, an object of the present invention is to solve the problems of the conventional apparatus. More specifically, an object of the present invention is to provide a high-temperature and high-pressure vessel provided with a chemical reaction promoting microwave supply device in which the restriction on the window is relaxed.
The present invention also provides a high-temperature and high-pressure vessel provided with a chemical reaction promoting microwave supply device capable of locally forming a high-temperature and high-pressure state and promoting the reaction by forming such a local reaction field. For the purpose.
[0006]
[Means for Solving the Problems]
The present invention includes a pressure vessel having a through hole, and a installed heat and corrosion resistance of the closed reaction vessel inside the pressure vessel, the distal end portion first window installation, hollow waveguide or coaxial line to The tip of the microwave supply device for promoting chemical reaction having the above-mentioned is inserted into the through-hole so as to be positioned in the pressure vessel, and the object to be heated is irradiated with the microwave through the waveguide or the coaxial line a high-temperature high-pressure vessel for, and a high-temperature high-pressure vessel, characterized in that a control means for equalizing the internal pressure of the reaction vessel and pressure vessel as gist.
[0007]
The above reaction vessel, [0008] which are summarized as high-temperature high-pressure vessel, characterized in that Ru closed reaction vessel der composed of a microwave-transparent material
The gist of the present invention is a high-temperature and high-pressure vessel characterized by comprising a second window installed in the middle of a waveguide or a coaxial line located outside the pressure vessel.
[0009]
In the present invention, a pressure sensor mounted in the pressure vessel is also mounted between the first window and the second window so that the internal pressure between the first window and the second window can be controlled. Preferably, the internal pressure between the first window and the second window is controlled to be equal to the internal pressure of the pressure vessel during the reaction under high temperature and high pressure conditions .
[0010]
The present invention, a plurality of the waveguide or coaxial line is introduced into a pressure vessel, uniformly an object to be heated having a large volume in the reaction vessel, and that they are to be heated to a wide range It is characterized by.
[0011]
In the present invention, a plurality of the waveguides or coaxial lines are arranged along the flow in the conduit as the pressure vessel, so that an object to be heated flowing in the reaction vessel can be continuously heated. It is characterized by that .
[0012]
Further, according to the present invention, the object to be heated in the container includes a high-temperature and high-pressure reaction system in which a microwave absorber and / or a microwave-absorbing catalyst are present, a high-temperature and high-pressure fluid system in a sub-supercritical state, and / or Alternatively, it is characterized by being an electrolytic reaction system, a photochemical reaction system, a reaction system using ultrasonic waves, or a reaction system using an external heating method .
[0013]
A temperature sensor and a pressure sensor are mounted in the container, and the microwave output is controlled based on the detection values of the sensors so that the pressure and temperature in the container can be maintained at set values.
[0014]
An observation window is attached to the container, which enables visual observation, fiberscope observation, and real-time spectroscopic measurement.
[0015]
Embodiment
A microwave supply device for promoting chemical reaction to a high-temperature and high-pressure vessel composed of a pressure vessel and a reaction vessel according to the present invention is characterized by having the following configuration.
Introducing a hollow waveguide or coaxial line into a pressure-resistant vessel that constitutes a high-temperature and high-pressure vessel, so that the opening can efficiently heat any position of the object to be heated in the reaction vessel by microwaves. .
Introducing a plurality of waveguides or coaxial lines into a pressure vessel so that a large-capacity object to be heated in the reaction vessel can be heated uniformly and over a wide range.
A plurality of waveguides or coaxial lines are arranged along the flow in the pipe so that the object to be heated flowing in the reaction vessel can be continuously heated.
To be able to accelerate the chemical reaction by heating to the supercritical state by microwave.
Use microwave heating and external heating together as the heating means.
A temperature sensor is installed in the reaction vessel, and a pressure sensor is installed in the pressure vessel, and the microwave output is controlled based on the detection values of these sensors so that the pressure and temperature in the high-temperature and high-pressure vessel can be maintained at the set values. thing.
Attach an observation window to the pressure vessel to enable visual and real-time spectroscopic measurement.
[0016]
(1) The high-temperature and high-pressure vessel is composed of a pressure-resistant vessel and a reaction vessel, and is provided with a heat-resistant and corrosion-resistant sealed reaction vessel inside the pressure-resistant vessel, and the internal pressures of the pressure-resistant vessel and the reaction vessel are equal. Therefore, the second window of the waveguide or coaxial line is basically not necessary.
(2) The waveguide or the coaxial line is provided with a first window as a partition window at the opening, and is preferably sealed by two partition windows. The first window is installed in the waveguide or coaxial line opening (in the microwave irradiating unit and the pressure vessel), and the second window is installed outside the vessel.
(3) The reaction vessel is a sealed reaction vessel made of a microwave permeable material (eg, quartz, tetrafluoroethylene, etc.).
(4) In the case of a continuous type, there is a sealed reaction vessel made of a microwave permeable substance in a metal pressure resistant vessel. The reaction vessel internal pressure and the pressure vessel internal pressure are controlled to be equal.
(5) the reactor is mainly heat and corrosion, the first window are primarily heat-pressure resistance (if there is a second window heat resistance only), the second window is mainly pressure resistance These are used properly and the restrictions are relaxed.
(6) In the reaction under the high temperature and high pressure conditions, the first window and the second window are set so that the pressure of the container (the internal pressure of the pressure vessel and the reaction vessel) and the pressure between the first window and the second window are equal. Control the pressure between.
As a result, since the pressure before and after the first window is equal, the structure of the first window can be applied to a thin sheet structure only by considering the structure mainly from the viewpoint of heat resistance and corrosion resistance. .
In addition, since the second window is installed outside the pressure vessel, the structure of the second window may be selected mainly from the viewpoint of pressure resistance.
In this way, by properly using the structure of the first window and the second window, the restriction of the window for the high-temperature and high-pressure vessel can be relaxed.
[0017]
(7) By considering the microwave penetration depth by the above method and selecting an appropriate frequency, only the vicinity of the opening can be locally heated.
(8) When there are two or more parts to be heated, introducing a plurality of the above-mentioned waveguides or coaxial lines into the pressure vessel, thereby increasing the capacity of the reaction vessel composed of the microwave permeable material. The object to be heated can be heated uniformly and over a wide range.
(8) In the case of a continuous (flow-through) reaction, the object to be heated flowing in the reaction vessel is continuously heated by attaching a plurality of the waveguides or coaxial lines to the pressure vessel at intervals. be able to.
(9) Additional steps such as cooling and solution introduction can be incorporated.
(10) The temperature unevenness of the object to be heated can be reduced by monitoring the temperature and controlling the microwave output.
[0018]
[Action]
In the high-temperature and high-pressure vessel of the present invention having the microwave supply device for promoting chemical reaction configured as described above, the first window only needs to consider heat resistance and corrosion resistance, and strength does not need to be considered. A thin sheet-like structure can be adopted, and the restriction of the window for the high-temperature and high-pressure vessel of high temperature and high pressure can be relaxed.
[0019]
Furthermore, the high-temperature and high-pressure vessel having the chemical reaction promoting microwave supply device of the present invention has the following actions and effects. An arbitrary position of the object to be heated can be efficiently heated by microwaves. It is possible to heat an object to be heated in large uniformly also a wide range. An object to be heated flowing in the pipeline can be continuously heated. The chemical reaction can be promoted by introducing microwaves into the high temperature / high pressure fluid system in the sub-supercritical state. The reaction process, yield, and reaction time can be improved. The reaction temperature can be kept constant, and the reaction status can be monitored visually or in real time.
By allowing the microwave absorber and / or the microwave absorbing catalyst to exist in the high temperature and high pressure reaction system, a high temperature and high pressure state can be locally formed. The reaction can be promoted by forming such a local reaction field.
[0020]
【Example】
Details of the present invention will be described in the examples. The present invention is not limited by these examples.
[0021]
Example 1
FIG. 1 shows a first embodiment of the present invention, and is a guide provided so that a tip portion is positioned in the container through a top plate of a pressure container of a high-temperature and high-pressure container composed of a pressure container and a reaction container. A first window (window 1) is provided at the insertion end of the wave tube or the coaxial line, the internal pressures of the pressure vessel and the reaction vessel are made equal, and the microwave oscillated by the microwave transmitter is passed through the waveguide or the coaxial line. An object to be heated in a reaction vessel made of a microwave permeable substance (quartz) is irradiated.
In this example, since there is no second window, the structure of the first window can be selected mainly from the viewpoint of heat resistance and pressure resistance.
[0022]
Example 2
FIG. 2 shows a second embodiment of the present invention, and is a guide provided so that the tip of the high-temperature high-pressure vessel composed of a pressure-resistant vessel and a reaction vessel passes through the top plate of the pressure-resistant vessel and is positioned in the vessel. A first window (window 1) is provided at the insertion end of the wave tube or the coaxial line, a second window (window 2) is provided in the other half of the waveguide or the coaxial line, and the inside of the pressure vessel and the waveguide are provided. It is configured to irradiate an object to be heated in a reaction vessel made of a microwave transmissive material (quartz) through a waveguide or a coaxial line with equal pressure and oscillated by a microwave transmitter. is there.
Therefore, in the reaction under the high temperature and high pressure conditions, if the pressure between the first window and the second window is controlled so that the pressure in the pressure vessel and the pressure between the first window and the second window become equal, Since the pressure before and after the window 1 becomes equal, the structure of the first window can be applied to a thin sheet structure only by considering the structure mainly from the viewpoint of heat resistance and corrosion resistance. Since the second window is installed outside the high-temperature and high-pressure container, the structure of the second window can be selected mainly from the viewpoint of pressure resistance.
[0023]
The waveguide or the coaxial line can be slidably attached to the top plate of the pressure vessel. In that case, a hollow waveguide or coaxial line is introduced into the pressure vessel, and its opening is close to the object to be heated (liquid or slurry) in the reaction container, so that an arbitrary position of the object to be heated can be efficiently It can be heated by microwaves, and only the catalyst part can be selectively heated in the catalytic reaction.
The opening is close to the object to be heated in the reaction vessel, and the vicinity of the opening can be locally heated by selecting an appropriate frequency in consideration of the penetration depth of the microwave.
[0024]
Example 3
3 and 4 show a third embodiment of the present invention, which is a high-temperature and high-pressure vessel in which a pipe line corresponding to a reaction vessel is concentrically arranged in a pipe line corresponding to a pressure vessel, and corresponds to a pressure vessel. A plurality of waveguides or coaxial lines are arranged along the flow so as to penetrate into the pipeline, and a first window is provided at an insertion end of the plurality of waveguides or coaxial lines, and the waveguides or coaxial lines are provided. A second window is provided in the middle of the line so that the pressure inside the pressure vessel and the inside of the waveguide (in the first window and the second window) are equal, and the microwave oscillated by the microwave transmitter is waveguided or coaxially. An object to be heated in a reaction vessel made of a microwave permeable substance is irradiated via a line.
Therefore, it is possible to continuously heat the liquid flowing in the pipe line corresponding to the reaction vessel, and additionally, a process such as a cooling device or a solution introduction can be taken in, and the thermometer T in the flow path. The temperature of the object to be heated can be maintained at a set value by monitoring the temperature by controlling the microwave output.
[0025]
【The invention's effect】
According to the present invention, it is possible to provide a high-temperature and high-pressure vessel having a chemical reaction promoting microwave supply device in which restrictions on windows in the high-temperature and high-pressure vessel are relaxed. Further, it is possible to provide a high-temperature and high-pressure vessel having a chemical reaction promoting microwave supply device that can form a high-temperature and high-pressure state locally and promote the reaction by forming such a local reaction field.
[Brief description of the drawings]
FIG. 1 is a conceptual diagram of a first embodiment of a high-temperature and high-pressure vessel having a microwave supply device for promoting chemical reaction according to the present invention.
FIG. 2 is a conceptual diagram of a second embodiment of a high-temperature high-pressure vessel having a microwave supply device for promoting chemical reaction according to the present invention.
FIG. 3 is a conceptual diagram of a third embodiment of a high-temperature high-pressure vessel having a microwave supply device for promoting chemical reaction according to the present invention.
FIG. 4 is a conceptual diagram of a third embodiment of a high-temperature high-pressure vessel having a microwave supply device for chemical reaction promotion according to the present invention.
[Explanation of symbols]
G Pressure gauge P Pressure pump T Thermometer V Pressure adjustment valve

Claims (13)

貫通口を有する耐圧容器と、耐圧容器の内側に設置された耐熱および耐食性の密閉式反応容器とを備え、先端第1の窓を設置した中空の導波管または同軸線路を有する化学反応促進用マイクロ波供給装置の前記先端部を前記貫通口に挿入して耐圧容器内に位置するように設けて導波管または同軸線路を介して被加熱物にマイクロ波を照射するための高温高圧容器であって耐圧容器と反応容器の内圧を等しくするための制御手段を設けたことを特徴とする高温高圧容器。Chemical reactions having a pressure-resistant container having a through hole, and a installed heat and corrosion resistance of the closed reaction vessel inside the pressure vessel, a hollow waveguide or coaxial line was installed first window at the distal end High temperature and high pressure for irradiating an object to be heated through a waveguide or a coaxial line by inserting the tip of the promoting microwave supply device into the through-hole to be positioned in the pressure vessel a container, high temperature and pressure vessel, characterized in that a control means for equalizing the internal pressure of the pressure vessel and the reaction vessel. さらに、先端部に第1の窓を設置した中空の導波管または同軸線路を有する化学反応促進用マイクロ波供給装置を備えることを特徴とする請求項1の高温高圧容器。 2. The high-temperature and high-pressure vessel according to claim 1, further comprising a chemical reaction promoting microwave supply device having a hollow waveguide or a coaxial line having a first window installed at the tip . 上記の反応容器が、マイクロ波透過性物質で構成された密閉式反応容器であることを特徴とする請求項1または2の高温高圧容器。The high-temperature and high-pressure vessel according to claim 1 or 2, wherein the reaction vessel is a sealed reaction vessel made of a microwave permeable material. 上記の導波管または同軸線路が耐圧容器の外側に位置する導波管または同軸線路の途中に設置した第2の窓を備えることを特徴とする請求項1、2または3の高温高圧容器。 4. The high-temperature and high-pressure vessel according to claim 1, wherein the waveguide or the coaxial line includes a second window installed in the middle of the waveguide or the coaxial line located outside the pressure-resistant vessel. . 上記の第1の窓と第2の窓の間の内圧と耐圧容器の内圧を等しくするための制御手段を設けたことを特徴とする請求項4の高温高圧容器。 5. The high-temperature and high-pressure vessel according to claim 4, further comprising control means for equalizing the internal pressure between the first window and the second window and the internal pressure of the pressure- resistant vessel. 高温高圧条件での反応時に第1の窓と第2の窓の間の内圧を耐圧容器の内圧と等しくなるように制御可能に構成したことを特徴とする請求項5の高温高圧容器。The first window and the high-temperature high-pressure container according to claim 5 in which the inner pressure between the second window and said controllably be configured to equal the pressure of the pressure vessel during the reaction at elevated temperature and pressure conditions. 上記の耐圧容器が、上記の導波管または同軸線路複数本導入するための貫通口を有することを特徴とする請求項1ないし6のいずれかの高温高圧容器。 Additional pressure vessel is one of high-temperature high-pressure container according to claim 1 to 6, characterized in that it has a through hole for a plurality of introducing the waveguide or coaxial line. 上記の耐圧容器が、液体を連続的に流通する管路であり、当該管路中に上記の複数本の導波管または同軸線路流れに沿って配置し、反応容器中を流通する被加熱物を連続的に加熱できるようにしたことを特徴とする請求項の高温高圧容器。 The pressure vessel is a conduit that continuously circulates liquid, and the plurality of waveguides or coaxial lines are arranged along the flow in the conduit, and the heated container that circulates in the reaction vessel 8. The high-temperature and high-pressure vessel according to claim 7 , wherein the product can be continuously heated. 上記の反応容器中の被加熱物がマイクロ波吸収体および/またはマイクロ波吸収性触媒を存在させた高温高圧反応系である請求項1ないし8のいずれかの高温高圧容器。Object to be heated in the reaction vessel described above, any of the high-temperature high-pressure container according to claim 1 to 8 is a high temperature high pressure reaction system was present microwave absorber and / or microwave absorbing catalyst. 上記の反応容器中の被加熱物が亜・超臨界状態にある高温高圧流体系である請求項1ないし9のいずれかの高温高圧容器。Any high-temperature high-pressure vessel of the object to be heated in the reaction vessel described above, claims 1 is a high-temperature high-pressure fluid systems in the sub-supercritical state 9. 上記の反応容器中の被加熱物が電解反応系、光化学反応系、超音波を用いた反応系および/または外部加熱法を用いた反応系である請求項1ないしのいずれかの高温高圧容器。 The high temperature and high pressure according to any one of claims 1 to 9 , wherein the object to be heated in the reaction vessel is an electrolytic reaction system, a photochemical reaction system, a reaction system using ultrasonic waves and / or a reaction system using an external heating method. container. 上記の反応容器に温度センサーおよび圧力センサー取付け、それらセンサーの検出値にもとづきマイクロ波出力を制御して反応容器内の圧力および温度を設定値に保持できるようにしたことを特徴とする請求項1ないし11のいずれかの高温高圧容器。 A temperature sensor and a pressure sensor are attached to the reaction vessel, and the microwave output is controlled based on detection values of the sensors so that the pressure and temperature in the reaction vessel can be maintained at set values. A high-temperature high-pressure vessel according to any one of 1 to 11. 上記の耐圧容器に観測用窓を取付け、目視、ファイバースコープによる観測およびリアルタイムでの分光計測を可能にしたことを特徴とする請求項1ないし12のいずれかの高温高圧容器。 The high-temperature and high-pressure vessel according to any one of claims 1 to 12, wherein an observation window is attached to the pressure-resistant vessel to enable visual observation, observation with a fiberscope, and real-time spectroscopic measurement.
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