JP2009148730A - Catalyst packing method into reactor and measuring-instrument fixing device - Google Patents

Catalyst packing method into reactor and measuring-instrument fixing device Download PDF

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JP2009148730A
JP2009148730A JP2007330851A JP2007330851A JP2009148730A JP 2009148730 A JP2009148730 A JP 2009148730A JP 2007330851 A JP2007330851 A JP 2007330851A JP 2007330851 A JP2007330851 A JP 2007330851A JP 2009148730 A JP2009148730 A JP 2009148730A
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reaction tube
reactor
measuring instrument
yarn
fixing
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JP5348880B2 (en
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Tomoki Fukui
友基 福井
Nobuo Momotomi
宣生 百冨
Masanori Nitta
正範 新田
Toshihiro Sato
俊裕 佐藤
Daisuke Tomikawa
大輔 富川
Toru Kuroda
徹 黒田
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Mitsubishi Rayon Co Ltd
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Mitsubishi Rayon Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a catalyst packing method which can position measuring instruments at a determined position in the longitudinal direction of a reactor without contacting the instruments to a wall of the reactor and therefor carry out smoothly packing of a catalyst into the reactor in such a state, and to provide a measuring instrument fixing device. <P>SOLUTION: Measuring instruments arranged with two threads is inserted into the reactor to be positioned at the determined position in the longitudinal direction of the reactor so that a part of one thread positions at the outer side of one opening of the reactor and a part of the other thread positions at the outer side of the other opening of the reactor, and also the catalyst is packed into the reactor in the state that two threads are tensed not to contact to the inner wall of the reactor. The measuring instrument fixing device 20, having this fixing means and a positioning means of the threads, is provided. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は、反応器への触媒の充填方法及び計測器固定装置に関する。   The present invention relates to a method for charging a catalyst into a reactor and a measuring instrument fixing device.

例えば、プロピレンからのアクロレインやアクリル酸、イソブチレンやtert−ブチルアルコールからのメタクロレインやメタクリル酸の工業的な製造では、固体酸化触媒の存在下に、原料を分子状酸素で気相接触酸化させる方法が広く利用されている。この気相接触酸化反応は、目的生成物が得られる反応と共に、反応温度が高すぎると逐次的に分解反応や酸化反応が生じてしまうおそれがある。また、気相接触酸化反応は発熱反応でもあり、目的生成物を高収率で得るには反応温度を厳密に制御する必要がある。   For example, in the industrial production of acrolein or acrylic acid from propylene, methacrolein or methacrylic acid from isobutylene or tert-butyl alcohol, a method of subjecting the raw material to vapor phase catalytic oxidation with molecular oxygen in the presence of a solid oxidation catalyst Is widely used. In this gas phase catalytic oxidation reaction, if the reaction temperature is too high, a decomposition reaction or an oxidation reaction may occur sequentially along with the reaction for obtaining the target product. Further, the gas phase catalytic oxidation reaction is also an exothermic reaction, and it is necessary to strictly control the reaction temperature in order to obtain a target product in a high yield.

気相接触酸化反応は、通常、数百〜数万本の反応管を有する多管式反応器により行われる。そして、反応温度の制御は、温度計測器により反応管内の温度を測定しながら、反応管の外部に循環させる熱媒により反応管壁を通して反応熱が除熱されることにより行われる。この温度計測器は、反応管内の所定の位置に設置される。ただし、反応管内の温度を正確に測定するためには、反応管に挿入された温度計測器が反応管の内壁に接触しないようにしなければならない。   The gas phase catalytic oxidation reaction is usually carried out by a multitubular reactor having hundreds to tens of thousands of reaction tubes. The reaction temperature is controlled by removing the heat of reaction through the reaction tube wall by a heat medium circulated outside the reaction tube while measuring the temperature in the reaction tube with a temperature measuring instrument. This temperature measuring device is installed at a predetermined position in the reaction tube. However, in order to accurately measure the temperature in the reaction tube, it is necessary to prevent the temperature measuring instrument inserted in the reaction tube from contacting the inner wall of the reaction tube.

反応管の内壁に接触しないように温度計測器を固定する方法としては、反応管内に挿入した際、計測器から反応管の内径方向に反応管壁に向かって突出し、かつその長さが反応管の内径とほぼ同等又は若干短い触れ止め部材を設けた温度計測器を用いる方法がある(特許文献1)。   As a method of fixing the temperature measuring device so as not to contact the inner wall of the reaction tube, when inserted into the reaction tube, it protrudes from the measuring device toward the inner diameter of the reaction tube toward the reaction tube wall, and its length is the reaction tube. There is a method of using a temperature measuring device provided with a touch-stop member that is approximately the same as or slightly shorter than the inner diameter of the above (Patent Document 1).

触れ止め部材を設けることにより、反応管の内壁に接触させることなく温度計測器を反応管内に固定できる。しかし、触れ止め部材を設けると、反応管に触媒を充填する際に触れ止め部材が障害となり、触媒が触れ止め部材の位置で詰まってしまうことがあった。
また、多管式反応器による反応では、反応管内の圧力損失を低くすることも重要であり、反応管内に圧力計測器が設けられることもあり、その場合にも同様の問題が生じることがある。
そのため、反応管内に挿入した各種計測器を、反応管の内壁に接触させずに、反応管の長さ方向の所定位置に位置させることができ、かつ反応管への触媒の充填が円滑に行えるような方策が望まれている。
特開2003−1094号公報
By providing the touch-stop member, the temperature measuring instrument can be fixed in the reaction tube without contacting the inner wall of the reaction tube. However, when the contact prevention member is provided, the contact prevention member becomes an obstacle when the reaction tube is filled with the catalyst, and the catalyst may be clogged at the position of the contact prevention member.
In the reaction using a multi-tubular reactor, it is also important to reduce the pressure loss in the reaction tube, and a pressure measuring device may be provided in the reaction tube. In this case, the same problem may occur. .
Therefore, various measuring instruments inserted into the reaction tube can be positioned at predetermined positions in the length direction of the reaction tube without contacting the inner wall of the reaction tube, and the catalyst can be smoothly charged into the reaction tube. Such a measure is desired.
JP 2003-1094 A

本発明は、反応器が有する反応管内に計測器を固定する際に、計測器を反応管の内壁に接触させずに、反応管の長さ方向の所定位置に位置させることができ、その状態で反応管への触媒の充填が円滑に行える反応器への触媒の充填方法、及び前記触媒の充填に利用できる計測器固定装置を提供する。   In the present invention, when the measuring instrument is fixed in the reaction tube of the reactor, the measuring instrument can be positioned at a predetermined position in the length direction of the reaction tube without contacting the inner wall of the reaction tube. The present invention provides a method of filling a catalyst into a reactor that can smoothly fill the catalyst into a reaction tube, and a measuring instrument fixing device that can be used for filling the catalyst.

本発明の反応器への触媒の充填方法は、反応器が有する反応管内に計測器を固定し、触媒を充填する方法であって、2本の糸条が取り付けられた計測器を、一方の糸条の一部が反応管の一方の開口よりも外側にあり、他方の糸条の一部が反応管の他方の開口よりも外側にあるように、反応管内に挿入し、前記計測器が反応管の長さ方向の所定位置に位置するように、かつ反応管の内壁に接触しないように、2本の糸条を緊張させた状態で、反応管内に触媒を充填する方法である。
また、本発明の反応器への触媒の充填方法は、前記反応器が複数の反応管を有している多管式反応器であって、計測器を固定する装置を、計測器を固定する反応管とは別の反応管の開口部の形状を利用して固定することが好ましい。
The catalyst filling method of the reactor of the present invention is a method in which a measuring instrument is fixed in the reaction tube of the reactor and the catalyst is filled, and the measuring instrument provided with two yarns is attached to one of the reactors. The measuring instrument is inserted into the reaction tube so that a part of the yarn is outside the one opening of the reaction tube and a part of the other yarn is outside the other opening of the reaction tube. In this method, the catalyst is filled in the reaction tube in a state where the two threads are tensioned so as to be positioned at a predetermined position in the length direction of the reaction tube and not to contact the inner wall of the reaction tube.
Further, the catalyst filling method of the reactor according to the present invention is a multi-tube reactor in which the reactor has a plurality of reaction tubes, and the device for fixing the measuring device is fixed to the measuring device. It is preferable to fix using the shape of the opening of the reaction tube different from the reaction tube.

本発明の計測器固定装置は、反応器が有する反応管内に計測器を固定する装置であって、前記計測器に取り付けられた2本の糸条のうち、一方の糸条の一部が反応管の一方の開口よりも外側にあるようにして、他方の糸条の一部を反応管の他方の開口よりも外側で、該糸条を緊張させた状態で固定する固定手段と、前記計測器が前記反応管の内壁に接触しないように、固定手段で固定された前記糸条の位置を決める位置決め手段とを有する。
また、前記反応器が複数の反応管を有している多管式反応器の反応管内に計測器を固定する装置であって、前記位置決め手段が、計測器を固定する反応管とは別の反応管の開口部の形状を利用して固定し、前記固定手段で固定された糸条の位置を決める手段であることが好ましい。
The measuring device fixing device of the present invention is a device for fixing a measuring device in a reaction tube of the reactor, and one of the two yarns attached to the measuring device reacts with one part of the yarn. A fixing means for fixing a part of the other yarn outside the other opening of the reaction tube in a tensioned state so as to be outside the one opening of the tube, and the measurement Positioning means for determining the position of the yarn fixed by the fixing means so that the vessel does not contact the inner wall of the reaction tube.
The reactor is a device for fixing a measuring instrument in a reaction tube of a multi-tube reactor having a plurality of reaction tubes, wherein the positioning means is different from the reaction tube for fixing the measuring device. It is preferably a means for fixing using the shape of the opening of the reaction tube and determining the position of the yarn fixed by the fixing means.

本発明の反応器への触媒の充填方法は、反応器が有する反応管内の長さ方向の所定位置に、反応管の内壁に接触させないようにして計測器を固定することができ、その状態で触媒を反応管内に円滑に充填できる。
また、本発明の計測器固定装置は、反応器が有する反応管内の長さ方向の所定位置に、反応管の内壁に接触させないように計測器を固定できる。
In the method of filling the catalyst in the reactor of the present invention, the measuring instrument can be fixed at a predetermined position in the length direction in the reaction tube of the reactor so as not to contact the inner wall of the reaction tube. The catalyst can be smoothly filled in the reaction tube.
Moreover, the measuring instrument fixing device of the present invention can fix the measuring instrument at a predetermined position in the length direction in the reaction tube of the reactor so as not to contact the inner wall of the reaction tube.

本発明の反応器への触媒の充填方法は、反応器が有する反応管内の所定位置に計測器を固定し、触媒を充填する方法である。
反応器は、反応管を有しているものであれば特に限定されない。例えば、プロピレンを気相接触酸化させてアクロレインやアクリル酸を得る反応や、イソブチレンやtert−ブチルアルコールを気相接触酸化させてメタクロレインやメタクリル酸を得る反応等に用いられる多管式反応器等が挙げられる。また、反応管を1本のみ有する反応管であってもよい。
このような多管式反応器としては、例えば、図1に示すような多管式反応器1が挙げられる。
The method of filling the catalyst into the reactor of the present invention is a method of filling the catalyst by fixing the measuring device at a predetermined position in the reaction tube of the reactor.
The reactor is not particularly limited as long as it has a reaction tube. For example, a multi-tubular reactor used in a reaction in which propylene is oxidized in a gas phase to obtain acrolein or acrylic acid, a reaction in which isobutylene or tert-butyl alcohol is oxidized in a gas phase to obtain methacrolein or methacrylic acid, etc. Is mentioned. Moreover, the reaction tube which has only one reaction tube may be sufficient.
An example of such a multitubular reactor is a multitubular reactor 1 as shown in FIG.

多管式反応器1は、下側チャンネル2と、シェル3と、上側チャンネル4とを有する。
シェル3の内部には、管板5a、5bが設けられ、該管板5a、5bには長尺の反応管6が複数本固定される。
反応管6の本数は多管式反応器により異なるが、通常、数百〜数万本である。これらの複数の反応管6は、各反応管6の温度を正確に制御しやすい点から、図4に示すように、規則的に配列されることが好ましい。
The multitubular reactor 1 has a lower channel 2, a shell 3, and an upper channel 4.
Inside the shell 3, tube plates 5a and 5b are provided, and a plurality of long reaction tubes 6 are fixed to the tube plates 5a and 5b.
The number of reaction tubes 6 varies depending on the multitubular reactor, but is usually several hundred to several tens of thousands. The plurality of reaction tubes 6 are preferably arranged regularly as shown in FIG. 4 because it is easy to accurately control the temperature of each reaction tube 6.

反応管6の長さは、通常1〜10m程度である。反応管6の長さが1m以上であれば、反応管6の本数を少なくし、反応管6毎の触媒充填斑、活性斑、熱媒による除熱程度の斑が生じるのを防ぐことでき、目的生成物の製造効率が向上する。また、反応管6の長さが10m以下であれば、反応時の反応管内の圧力損失を小さくすることができ、反応ガスの供給動力を抑えることができ経済的である。また、反応管6の内径は、通常20〜30mm程度である。   The length of the reaction tube 6 is usually about 1 to 10 m. If the length of the reaction tube 6 is 1 m or more, the number of reaction tubes 6 can be reduced, and catalyst-packed spots, active spots, and spots of heat removal by the heat medium for each reaction tube 6 can be prevented. The production efficiency of the target product is improved. If the length of the reaction tube 6 is 10 m or less, the pressure loss in the reaction tube during the reaction can be reduced, and the supply power of the reaction gas can be suppressed, which is economical. Moreover, the internal diameter of the reaction tube 6 is about 20-30 mm normally.

また、図3に示すように、目開き1〜2mm程度の金網9aと、反応管6の開口6aに相当する位置に開口を有するパンチングプレート9bとが、ボルト9cにより管板5aに取り付けられる。そして、反応管6に触媒が充填されることにより触媒層7が形成される。   As shown in FIG. 3, a wire mesh 9a having an opening of about 1 to 2 mm and a punching plate 9b having an opening at a position corresponding to the opening 6a of the reaction tube 6 are attached to the tube plate 5a by bolts 9c. Then, the catalyst layer 7 is formed by filling the reaction tube 6 with the catalyst.

シェル3内部の反応管6の外側の部分には、熱媒が流される。熱媒は、図1に示すように、シェル3に設けられた下側熱媒ノズル3aからシェル3内部へと導かれ、上側熱媒ノズル3bから流出される。熱媒は、亜硝酸ナトリウム、硝酸ナトリウム、及び硝酸カリウムの混合物等が使用される。   A heat medium is caused to flow through the outer portion of the reaction tube 6 inside the shell 3. As shown in FIG. 1, the heat medium is guided from the lower heat medium nozzle 3a provided in the shell 3 into the shell 3, and flows out from the upper heat medium nozzle 3b. As the heat medium, a mixture of sodium nitrite, sodium nitrate, and potassium nitrate is used.

下側チャンネル2には下側ノズル2aが設けられ、上側チャンネル4には上側ノズル4aが設けられる。反応ガスは下側ノズル2aから多管式反応器1内に供給され、下側チャンネル2内で各反応管6に分配され、予熱されて触媒層7内で反応する。この反応により生じる反応熱は、反応管6の外側に流されている熱媒によって反応管壁を通して取り除かれ、反応管6内が所定の温度に調節される。反応管6を通過してきた反応ガスは、上側チャンネル4に設けられた上側ノズル4aから次工程に送られる。   The lower channel 2 is provided with a lower nozzle 2a, and the upper channel 4 is provided with an upper nozzle 4a. The reaction gas is supplied from the lower nozzle 2 a into the multi-tube reactor 1, is distributed to the reaction tubes 6 in the lower channel 2, is preheated, and reacts in the catalyst layer 7. The reaction heat generated by this reaction is removed through the reaction tube wall by the heat medium flowing outside the reaction tube 6, and the inside of the reaction tube 6 is adjusted to a predetermined temperature. The reaction gas that has passed through the reaction tube 6 is sent to the next process from the upper nozzle 4 a provided in the upper channel 4.

下側チャンネル2は、反応ガスを各反応管6へと分配する働きをし、上側チャンネル4は反応管6から出てくる反応ガスを収集する働きをする。多管式反応器1に流す反応ガスの向きを上下逆にする場合には、下側チャンネル2と上側チャンネル4の働きが逆になる。   The lower channel 2 serves to distribute the reaction gas to each reaction tube 6, and the upper channel 4 serves to collect the reaction gas exiting from the reaction tube 6. When the direction of the reaction gas flowing through the multi-tube reactor 1 is turned upside down, the functions of the lower channel 2 and the upper channel 4 are reversed.

気相接触酸化反応は、分解反応や酸化反応が逐次的に起きることを防ぐために、反応温度を厳密に制御する必要がある。そのため、温度計測器10により反応管6内の温度が測定される。温度計測器10は、工業的に使用できるものであればよく、通常、熱伝対または抵抗温度計が使用される。   In the gas phase catalytic oxidation reaction, it is necessary to strictly control the reaction temperature in order to prevent the decomposition reaction and the oxidation reaction from occurring sequentially. Therefore, the temperature in the reaction tube 6 is measured by the temperature measuring instrument 10. The temperature measuring instrument 10 may be any industrially usable one, and a thermocouple or a resistance thermometer is usually used.

温度計測器10の反応管6に固定した状態で触媒を充填する手法は、計測器固定装置を用いることにより容易に行うことができる。以下、本発明の計測器固定装置の実施形態の一例を図2に示し、詳細に説明する。
[計測器固定装置]
本発明の計測器固定装置20は、(1)温度計測器10に取り付けた糸条21の一部を、反応管6の開口6bよりも外側で、糸条21を緊張させた状態で固定する固定手段と、(2)温度計測器10が反応管6の内壁に接触しないように、糸条21の位置を決める位置決め手段とを有する。
The method of filling the catalyst while being fixed to the reaction tube 6 of the temperature measuring device 10 can be easily performed by using a measuring device fixing device. Hereinafter, an example of an embodiment of the measuring instrument fixing device of the present invention will be described in detail with reference to FIG.
[Measurement fixing device]
The measuring instrument fixing device 20 of the present invention (1) fixes a part of the yarn 21 attached to the temperature measuring instrument 10 outside the opening 6b of the reaction tube 6 in a state where the yarn 21 is tensioned. And (2) positioning means for determining the position of the yarn 21 so that the temperature measuring instrument 10 does not contact the inner wall of the reaction tube 6.

計測器固定装置20は、図2に示すように、糸条21、22と、管状部材24と、固定部材25とを有している。ただし、本発明における糸条とは、糸状の細長い形態を有し、温度計測器に取り付けて緊張させることにより、反応管内において温度計測器を所望の位置に固定するものである。本発明の糸条の断面積は、反応管内部の断面積に対して1/5以下であり、断面形状は特に限定されない。
糸条21の材質としては、ステンレス、鉄、樹脂等を用いることができる。特に好ましい糸条21は、耐久性及び反応への影響等の点からステンレスワイヤーである。
温度計測器10への糸条21の取り付けは、特に限定されないが、例えば、溶接で固定することができる。
As shown in FIG. 2, the measuring instrument fixing device 20 includes yarns 21 and 22, a tubular member 24, and a fixing member 25. However, the yarn in the present invention has a thread-like elongated shape, and is fixed to a desired position in the reaction tube by attaching and tensioning the temperature measuring instrument. The cross-sectional area of the yarn of the present invention is 1/5 or less of the cross-sectional area inside the reaction tube, and the cross-sectional shape is not particularly limited.
As the material of the yarn 21, stainless steel, iron, resin, or the like can be used. A particularly preferable yarn 21 is stainless steel wire from the viewpoint of durability and influence on reaction.
The attachment of the yarn 21 to the temperature measuring instrument 10 is not particularly limited, but can be fixed by welding, for example.

糸条22については、温度計測器10の導線部11を糸条22として用いることが好ましい。また、糸条21と同じものを新たに温度計測器10に取り付けて糸条22としてもよい。
温度計測器10に取り付けられた糸条22は、反応管6の開口6aよりも外側にある部分が多管式反応器1に固定される。糸条22が固定される場所は、糸条21と糸条22を緊張させて温度計測器10を所定位置に位置させることができる場所であればよい。例えば、糸条22の反応管6の開口6aよりも外側にある部分を、金網9a、パンチングプレート9bと共に管板5aに固定することが挙げられる。また、金網9aの開口6aの位置に相当する部分に糸条22の自由端が直接固定されていてもよく、開口6a側の反応管6内で固定されていてもよい。
また、温度計測器10の導線部11を糸条22として使用する場合には、図3に示すように、糸条22の反応管6の開口6aよりも外側にある部分が、金網9a、パンチングプレート9bと共にボルト9c等を用いて管板5aに固定され、さらに多管式反応器1の外側に導かれているのがよい。
温度計測器10を複数の反応管6に設置する場合は、それらの糸条22を束ねて一箇所に固定してもよく、温度計測器10の本数が多い場合には、ある程度まとめて複数箇所で固定してもよい。
For the yarn 22, it is preferable to use the conducting wire portion 11 of the temperature measuring instrument 10 as the yarn 22. Alternatively, the same yarn 21 may be newly attached to the temperature measuring instrument 10 as the yarn 22.
The yarn 22 attached to the temperature measuring instrument 10 is fixed to the multi-tube reactor 1 at a portion outside the opening 6 a of the reaction tube 6. The place where the yarn 22 is fixed may be any place where the temperature measuring device 10 can be positioned at a predetermined position by tensioning the yarn 21 and the yarn 22. For example, fixing the portion of the yarn 22 outside the opening 6a of the reaction tube 6 to the tube plate 5a together with the wire mesh 9a and the punching plate 9b can be mentioned. Further, the free end of the yarn 22 may be directly fixed to a portion corresponding to the position of the opening 6a of the wire mesh 9a, or may be fixed in the reaction tube 6 on the opening 6a side.
Further, when the conductor portion 11 of the temperature measuring instrument 10 is used as the yarn 22, as shown in FIG. 3, the portion of the yarn 22 outside the opening 6a of the reaction tube 6 is a wire mesh 9a, punching. It is preferable that the plate 9b is fixed to the tube plate 5a by using bolts 9c and the like and further led to the outside of the multi-tube reactor 1.
When the temperature measuring device 10 is installed in a plurality of reaction tubes 6, the yarns 22 may be bundled and fixed in one place. When the number of the temperature measuring devices 10 is large, the temperature measuring device 10 is gathered to some extent. It may be fixed with.

計測器固定装置20には、図2に示すように、(1)の固定手段である固定部材25が、計測器固定装置本体23に設けられている。固定部材25は、温度計測器10に取り付けた糸条21の一部、好ましくは自由端21aを固定でき、糸条21を引っ張ることにより、糸条21、22を緊張した状態にできるものであればよい。
例えば、図2に示すように、計測器固定装置本体上部23aに下から上にボルト状の固定部材25を設置し、糸条21の自由端21aを固定し、該ボルト状の固定部材25を締めていくことにより糸条21を引っ張るようにすればよい。また、固定部材25の糸条21を固定する部分をフックにしてもよい。また、固定部材25は、糸条21の自由端21aを固定して、糸条21を巻き取ることのできる構造としてもよい。
As shown in FIG. 2, the measuring device fixing device 20 is provided with a fixing member 25 as a fixing means (1) in the measuring device fixing device main body 23. The fixing member 25 can fix a part of the yarn 21 attached to the temperature measuring instrument 10, preferably the free end 21 a, and pull the yarn 21 to make the yarns 21 and 22 in a tensioned state. That's fine.
For example, as shown in FIG. 2, a bolt-shaped fixing member 25 is installed on the measuring instrument fixing device main body upper portion 23a from the bottom to the top, the free end 21a of the yarn 21 is fixed, and the bolt-shaped fixing member 25 is fixed. The yarn 21 may be pulled by tightening. Moreover, you may make the part which fixes the thread 21 of the fixing member 25 into a hook. Further, the fixing member 25 may have a structure in which the free end 21a of the yarn 21 is fixed and the yarn 21 can be wound up.

固定部材25の材質としては、ステンレス、鉄等の金属、樹脂、木等が挙げられ、耐久性、強度、経済性の点から鉄製であるのが好ましい。   Examples of the material of the fixing member 25 include metals such as stainless steel and iron, resin, wood, and the like, and iron is preferable from the viewpoint of durability, strength, and economy.

また、計測器固定装置本体23には、図2に示すように、管状部材24が設けられている。管状部材24は、本体24aの内部が空洞となっており、触媒を投入するための開口24bが設けられている。管状部材24の形状は、特に限定されず、例えば、反応管6の内径より大きな本体24aに、絞り部24cを設け、さらに絞り部24cから突出するように先端部24dが形成されている形状が挙げられる。先端部24dの径は反応管6の内径よりも小さく、開口6bから反応管6内に挿入できるようになっている。管状部材24の本体24aは、円筒形であっても角柱形であってもよく、限定はない。
管状部材24は、計測器固定装置本体23に完全に固定されていても、計測器固定装置本体23を固定した状態で鉛直方向または水平方向に移動させて位置を微調整できるようになっていてもよい。
Further, the measuring instrument fixing device main body 23 is provided with a tubular member 24 as shown in FIG. The tubular member 24 is hollow inside the main body 24a, and is provided with an opening 24b for introducing a catalyst. The shape of the tubular member 24 is not particularly limited, and for example, a shape in which a throttle portion 24c is provided in a main body 24a larger than the inner diameter of the reaction tube 6 and a tip portion 24d is formed so as to protrude from the throttle portion 24c. Can be mentioned. The diameter of the tip 24d is smaller than the inner diameter of the reaction tube 6 and can be inserted into the reaction tube 6 through the opening 6b. The main body 24a of the tubular member 24 may be cylindrical or prismatic, and is not limited.
Even if the tubular member 24 is completely fixed to the measuring instrument fixing device main body 23, the tubular member 24 can be moved in the vertical direction or the horizontal direction in a state where the measuring instrument fixing device main body 23 is fixed, so that the position can be finely adjusted. Also good.

また、計測器固定装置20は、(2)の位置決め手段も有する。計測器固定装置本体23の側部23b、23c(以下、側部23b、23cとする。)の先端部を、温度計測器10を設置する反応管6とは別の反応管6(図2では隣の反応管6)に挿入し、固定したときに、管状部材24の先端部24dと固定部材25とが温度計測器10を設置する反応管6の開口6bの位置に配置される。この状態で糸条21を管状部材24の内部を通過させて固定部材25に固定することにより、糸条21の位置決めができる。
前記側部23a、23cを挿入して固定する別の反応管とは、糸条21の位置決めができる範囲であればいずれの反応管6であってもよく、位置決めが容易で精度が高くなる点から、温度計測器10を設置する反応管6から数本以内に位置する反応管6であることが好ましい。
Moreover, the measuring instrument fixing device 20 also has a positioning means (2). The reaction tube 6 (in FIG. 2) is different from the reaction tube 6 on which the temperature measuring device 10 is installed at the tip of the side portions 23 b and 23 c (hereinafter referred to as side portions 23 b and 23 c) of the measuring instrument fixing device main body 23. When inserted into the adjacent reaction tube 6) and fixed, the distal end 24d of the tubular member 24 and the fixing member 25 are arranged at the position of the opening 6b of the reaction tube 6 where the temperature measuring instrument 10 is installed. In this state, the yarn 21 can be positioned by passing the inside of the tubular member 24 and fixing it to the fixing member 25.
The other reaction tube for inserting and fixing the side portions 23a and 23c may be any reaction tube 6 as long as the yarn 21 can be positioned, and positioning is easy and accuracy is high. Therefore, it is preferable that the reaction tube 6 is located within several tubes from the reaction tube 6 in which the temperature measuring device 10 is installed.

側部23b、23cの先端部は、反応管6の内壁に直接固定できるような構造であってもよく、側部23b、23cを挿入する反応管6に予め触媒を充填しておき、該触媒内に差し込むことにより固定できるような構造であってもよい。また、例えば、反応管6の開口部6bが管板5bより上に出ているような多管式反応管の場合等、そのような反応管の開口部の形状や管板の形状を利用して固定できるような側部23b、23cであってもよい(図5)。また、計測器固定装置の側部の本数は2本には限られず、1本であってもよく、3本以上であってもよい。例えば、図4に示すように、反応管6Aに温度計測器を固定する場合に、領域a、b、cの部分にある反応管6及び管板5bの形状を利用して装置を固定できる3本の側部を有し、それら3本の側部が正四面体状に設置されることにより固定部材が反応管6A上に配置されるような計測器固定装置であってもよい。
また、反応管が1本のみである反応器に対して温度計測器を固定して触媒の充填を行う場合等は、側部23b、23cを管板5b上に固定して糸条21の位置決めが行える計測器固定装置であってもよい。
The ends of the side portions 23b and 23c may be structured to be directly fixed to the inner wall of the reaction tube 6, and the reaction tube 6 into which the side portions 23b and 23c are inserted is previously filled with a catalyst, The structure which can be fixed by inserting in may be sufficient. In addition, for example, in the case of a multi-tube reaction tube in which the opening 6b of the reaction tube 6 protrudes above the tube plate 5b, the shape of the opening of the reaction tube or the shape of the tube plate is used. The side portions 23b and 23c may be fixed (FIG. 5). Further, the number of side portions of the measuring instrument fixing device is not limited to two, and may be one or three or more. For example, as shown in FIG. 4, when a temperature measuring instrument is fixed to the reaction tube 6A, the apparatus can be fixed using the shapes of the reaction tube 6 and the tube plate 5b in the regions a, b, and c. It may be a measuring instrument fixing device having a side portion of a book and arranging the three side portions in a regular tetrahedron shape so that the fixing member is arranged on the reaction tube 6A.
When the temperature measuring instrument is fixed to a reactor having only one reaction tube and the catalyst is charged, etc., the side portions 23b and 23c are fixed on the tube plate 5b and the yarn 21 is positioned. It may be a measuring instrument fixing device capable of performing the above.

[反応器への触媒の充填方法]
以下、本発明の、反応管6に温度計測器10を固定して触媒を充填する方法について説明するが、本発明の方法はこれに限定されない。尚、温度計測器10が、圧力計測器であっても、反応管6への固定及び触媒の充填は同様の方法で行うことができる。
[Method of filling catalyst into reactor]
Hereinafter, although the method of fixing the temperature measuring device 10 to the reaction tube 6 and filling the catalyst of the present invention will be described, the method of the present invention is not limited to this. In addition, even if the temperature measuring device 10 is a pressure measuring device, the fixing to the reaction tube 6 and the filling of the catalyst can be performed by the same method.

本発明では、図2に示すように、温度計測器10に2本の糸条21、22を取り付け、糸条21の一部が反応管6の開口6bよりも外側にあり、糸条22の一部が反応管6の開口6aよりも外側にあるように、温度計測器10を反応管6内に挿入する。
これらの反応管6への挿入方法としては、糸条21、温度計測器10、糸条22が繋がった状態のものをこの順に、反応管6の開口6aの内径方向の中心部分に対応する、金網9aの部分から挿入していく方法が好ましい。
In the present invention, as shown in FIG. 2, two yarns 21 and 22 are attached to the temperature measuring device 10, and a part of the yarn 21 is outside the opening 6 b of the reaction tube 6. The temperature measuring instrument 10 is inserted into the reaction tube 6 so that a part is outside the opening 6 a of the reaction tube 6.
As a method for inserting these into the reaction tube 6, the one in which the yarn 21, the temperature measuring device 10, and the yarn 22 are connected corresponds to the central portion in the inner diameter direction of the opening 6 a of the reaction tube 6 in this order. The method of inserting from the part of the metal mesh 9a is preferable.

ついで、糸条21、22を緊張させた状態に保つことにより、温度計測器10を反応管6の長さ方向の所定位置に位置させる。糸条21及び22を緊張させた状態にする方法としては、例えば、以下に示す方法が挙げられる。   Next, the temperature measuring device 10 is positioned at a predetermined position in the length direction of the reaction tube 6 by keeping the yarns 21 and 22 in a tensioned state. Examples of a method for bringing the yarns 21 and 22 into a tensioned state include the following methods.

糸条21の反応管6の開口6bよりも外側にある部分は、計測器固定用装置20の管状部材24内を通過させ、固定部材25に固定する。糸条21の計測器固定装置20への固定は、糸条21の自由端21aにて行うのが好ましい。また、管状部材24の先端部24dが温度計測器10を挿入した反応管6内に開口6bから挿入され、その上方に固定部材25が位置されるように、計測器固定用装置20の側部23b、23cの先端部を、温度計測器10を挿入した反応管6とは別の反応管6(図2では隣の反応管6)内に挿入して固定する。   A portion of the yarn 21 outside the opening 6 b of the reaction tube 6 passes through the tubular member 24 of the measuring instrument fixing device 20 and is fixed to the fixing member 25. The yarn 21 is preferably fixed to the measuring device fixing device 20 at the free end 21 a of the yarn 21. Further, the side portion of the measuring instrument fixing device 20 is arranged such that the distal end 24d of the tubular member 24 is inserted into the reaction tube 6 into which the temperature measuring instrument 10 is inserted from the opening 6b, and the fixing member 25 is positioned above the opening 6b. The tip portions of 23b and 23c are inserted and fixed in a reaction tube 6 (an adjacent reaction tube 6 in FIG. 2) different from the reaction tube 6 in which the temperature measuring instrument 10 is inserted.

また、糸条22を固定する方法は、糸条21と糸条22を緊張させて温度計測器10を所定位置に位置させることができれば特に限定されない。例えば、図3に示すように、糸条22の反応管6の開口6aよりも外側にある部分を、金網9a及びパンチングプレート9bと共にボルト9cにより管板5aに固定する方法が挙げられる。また、金網9aの開口6aの位置に相当する部分に糸条22の自由端を直接固定する方法であってもよく、開口6a側の反応管6内で固定する方法であってもよい。
温度計測器10の導線部11を糸条22として用いる場合には、糸条22である導線部11の、反応管6の開口6aよりも外側にある部分を、金網9a及びパンチングプレート9bと共にボルト9cにより管板5aに固定し、さらに計測器用ノズル2bから多管式反応器1の外側に導けばよい。
温度計測器10を複数の反応管6に固定して糸条22が複数本ある場合には、それらを束ねて一箇所に固定してもよく、数が多い場合にはある程度まとめたものを複数箇所に固定してもよい。
Moreover, the method of fixing the yarn 22 is not particularly limited as long as the yarn 21 and the yarn 22 are tensioned and the temperature measuring device 10 can be positioned at a predetermined position. For example, as shown in FIG. 3, there is a method in which a portion of the yarn 22 outside the opening 6a of the reaction tube 6 is fixed to the tube plate 5a by a bolt 9c together with a wire mesh 9a and a punching plate 9b. Alternatively, the free end of the yarn 22 may be directly fixed to the portion corresponding to the position of the opening 6a of the wire mesh 9a, or may be fixed in the reaction tube 6 on the opening 6a side.
When the lead wire portion 11 of the temperature measuring instrument 10 is used as the yarn 22, the portion of the lead wire portion 11 that is the yarn 22 outside the opening 6a of the reaction tube 6 is bolted together with the wire mesh 9a and the punching plate 9b. It may be fixed to the tube plate 5a by 9c, and further guided outside the multi-tube reactor 1 from the measuring instrument nozzle 2b.
When the temperature measuring device 10 is fixed to a plurality of reaction tubes 6 and there are a plurality of yarns 22, they may be bundled and fixed in one place. It may be fixed in place.

ついで、例えば、図2に示すような糸条21を固定したボルト状の固定部材25を、上方に締め上げることにより、糸条21を計測器固定装置20側へと引っ張る。糸条21を引っ張ることにより、糸条22がボルト9cによって固定されているために、糸条21及び糸条22が緊張した状態となる。そのため、糸条21及び糸条22の長さを調整することにより温度計測器10を反応管6内の所定位置に位置させることができる。また、糸条21及び糸条22を緊張させた状態で、温度計測器10を、反応管6の内壁に接触させないように位置させることができる。このとき、計測器固定装置20の管状部材先端部24d及び固定部材25を反応管6の内径方向の中心軸上に位置させることにより、温度計測器10が反応管6の内径方向の中心に位置されることが好ましい。   Next, for example, by tightening a bolt-shaped fixing member 25 to which the yarn 21 is fixed as shown in FIG. 2 upward, the yarn 21 is pulled toward the measuring instrument fixing device 20. By pulling the yarn 21, since the yarn 22 is fixed by the bolt 9c, the yarn 21 and the yarn 22 are in a tensioned state. Therefore, the temperature measuring device 10 can be positioned at a predetermined position in the reaction tube 6 by adjusting the lengths of the yarn 21 and the yarn 22. Further, the temperature measuring device 10 can be positioned so as not to contact the inner wall of the reaction tube 6 in a state where the yarn 21 and the yarn 22 are in tension. At this time, the temperature measuring instrument 10 is positioned at the center in the inner diameter direction of the reaction tube 6 by positioning the tubular member tip 24d and the fixing member 25 of the measuring instrument fixing device 20 on the center axis in the inner diameter direction of the reaction tube 6. It is preferred that

触媒の充填は、このように、糸条21、22を緊張させて温度計測器10を反応管6内に位置させた状態で、計測器固定装置20の管状部材24の開口24bから触媒を投入することにより行う。開口24bから投入された触媒は、管状部材24の先端部24dから反応管6に充填される。   In this way, the catalyst is charged through the opening 24b of the tubular member 24 of the measuring instrument fixing device 20 in such a state that the yarns 21 and 22 are tensioned and the temperature measuring instrument 10 is positioned in the reaction tube 6. To do. The catalyst charged from the opening 24 b is filled into the reaction tube 6 from the tip 24 d of the tubular member 24.

反応管6内に充填する触媒は、1種であっても、2種以上であってもよい。
触媒としては、固体触媒が使用でき、例えば、モリブデン、ビスマスを含む複合酸化物等の固体酸化触媒等が挙げられる。また、触媒は、触媒以外に反応に関与しない不活性な粒子を含んでいても構わない。
The catalyst filled in the reaction tube 6 may be one type or two or more types.
As the catalyst, a solid catalyst can be used, and examples thereof include a solid oxidation catalyst such as a composite oxide containing molybdenum and bismuth. Moreover, the catalyst may contain inactive particles that do not participate in the reaction other than the catalyst.

糸条21、22を緊張させる操作は、温度計測器10を所定の位置に位置させることができる範囲内であれば、触媒をある程度充填させた後であってもかまわない。
計測器固定装置20は、触媒の充填後に、糸条21を切断することにより取り外すことができる。
The operation of tensioning the yarns 21 and 22 may be performed after the catalyst is filled to some extent as long as the temperature measuring device 10 can be positioned at a predetermined position.
The measuring instrument fixing device 20 can be removed by cutting the yarn 21 after filling the catalyst.

温度計測器10は、少なくとも1つ以上の反応管6に設置すればよく、反応管6内の温度を高精度に調節する点から、図1のように、反応管6の長さ方向の位置がそれぞれ異なるように、複数の反応管6に温度計測器10を設置することが好ましい。また、例えば、2種以上の活性の異なる触媒を同一の反応管6内に2層に分けて充填する場合等、同一の反応管内に複数の温度計測器10を設けてもよい。   The temperature measuring device 10 may be installed in at least one or more reaction tubes 6, and from the point of adjusting the temperature in the reaction tube 6 with high accuracy, as shown in FIG. It is preferable to install the temperature measuring devices 10 in the plurality of reaction tubes 6 so that they are different from each other. In addition, for example, when two or more kinds of catalysts having different activities are packed in two layers in the same reaction tube 6, a plurality of temperature measuring devices 10 may be provided in the same reaction tube.

温度計測器10を複数設置する場合は、温度計測器10の、反応管6の長さ方向の設置間隔は0.1〜2mとするのが好ましい。
温度計測器10の設置間隔を2m以下とすれば、反応管内の正確な温度分布を測定することが容易になり、ホットスポット部の位置および温度を把握するのが容易になる。
また、多管式反応器では、反応管6内に設置した温度計測器10と同じ高さで、熱媒中に熱媒温度を測定する温度計測器を設けることが好ましい。そのため、温度計測器10の設置間隔を0.1m以下とすれば熱媒中の温度計測器の数も多くなり、装置コストが高くなるだけでなく、熱媒の流れを妨げてしまうおそれがある。
In the case where a plurality of temperature measuring devices 10 are installed, the installation interval of the temperature measuring devices 10 in the length direction of the reaction tube 6 is preferably 0.1 to 2 m.
If the installation interval of the temperature measuring device 10 is 2 m or less, it becomes easy to measure an accurate temperature distribution in the reaction tube, and it becomes easy to grasp the position and temperature of the hot spot portion.
Further, in the multi-tube reactor, it is preferable to provide a temperature measuring device for measuring the temperature of the heating medium in the heating medium at the same height as the temperature measuring device 10 installed in the reaction tube 6. Therefore, if the installation interval of the temperature measuring device 10 is 0.1 m or less, the number of temperature measuring devices in the heat medium increases, which not only increases the cost of the apparatus but also may hinder the flow of the heat medium. .

以上説明した、本発明の反応器への触媒の充填方法は、計測器を反応管内に固定する際、反応管の内壁に接触させることなく、反応管の長さ方向の所定の位置に固定できる。また、計測器には、触れ止め部材等の触媒の充填の障害になるものがないため、触媒の充填が円滑に行える。
また、本発明の計測器固定装置20を用いれば、このような多管式反応器に計測器を固定して触媒の充填する作業を容易に行うことができる。
As described above, the method of filling the catalyst into the reactor of the present invention can be fixed at a predetermined position in the length direction of the reaction tube without contacting the inner wall of the reaction tube when the measuring device is fixed in the reaction tube. . Moreover, since there is no obstacle to the filling of the catalyst such as a touch-stop member, the measuring device can smoothly fill the catalyst.
Further, by using the measuring instrument fixing device 20 of the present invention, it is possible to easily perform the work of fixing the measuring instrument to such a multi-tubular reactor and filling the catalyst.

尚、本発明の触媒の充填方法は、図2に例示した方法に限定されるものではない。
例えば、計測器固定装置20の固定方法は、計測器を固定する反応管6とは別の反応管6に挿入して固定する方法に限定されず、計測器を所定の位置に位置させることができる方法であれば、前記別の反応管6の開口部6bの形状や管板5bの形状を利用して固定できる側部を有する計測器固定装置を用いた別の固定方法であってもよい。
また、糸条21は、計測器固定装置20における管状部材24の先端部24dに取り付け、開口6b側の反応管6内で固定するようにしても構わない。
また、計測器固定装置20を、管板5a側に固定できるような構造とし、糸条22が反応管6の開口6bよりも外側にあるように温度計測器10を挿入し、糸条22の開口6bよりも外側の部分を管板5b上に固定する方法であってもよい。
また、計測器固定装置20も図2に示したものに限定されず、管状部材24及び固定部材25は、計測器を反応管内の所定位置に位置させることができるものであればよい。また、管状部材24及び固定部材25は、計測器固定装置本体23のいずれの部位に設置されていてもよく、例えば、管状部材24の上部に滑車を設け、固定部材25を側部23bに設置して、固定部材25が糸条21を水平方向に引っ張るような計測器固定装置20としてもよい。
The catalyst filling method of the present invention is not limited to the method illustrated in FIG.
For example, the fixing method of the measuring instrument fixing device 20 is not limited to the method of inserting and fixing the measuring instrument into a reaction tube 6 different from the reaction tube 6 fixing the measuring instrument, and the measuring instrument can be positioned at a predetermined position. As long as it can be used, another fixing method using a measuring instrument fixing device having a side part that can be fixed using the shape of the opening 6b of the other reaction tube 6 or the shape of the tube plate 5b may be used. .
Further, the yarn 21 may be attached to the distal end portion 24d of the tubular member 24 in the measuring instrument fixing device 20 and fixed in the reaction tube 6 on the opening 6b side.
Further, the measuring instrument fixing device 20 is structured to be fixed to the tube plate 5 a side, the temperature measuring instrument 10 is inserted so that the yarn 22 is outside the opening 6 b of the reaction tube 6, and the yarn 22 A method of fixing a portion outside the opening 6b on the tube plate 5b may be used.
Further, the measuring instrument fixing device 20 is not limited to that shown in FIG. 2, and the tubular member 24 and the fixing member 25 may be anything as long as the measuring instrument can be positioned at a predetermined position in the reaction tube. Further, the tubular member 24 and the fixing member 25 may be installed in any part of the measuring instrument fixing device main body 23. For example, a pulley is provided on the upper part of the tubular member 24, and the fixing member 25 is installed on the side portion 23b. And it is good also as the measuring device fixing device 20 in which the fixing member 25 pulls the thread | yarn 21 in a horizontal direction.

一般に使用される多管式反応器1に温度計測器を固定した様子を示した側断面図である。It is the sectional side view which showed a mode that the temperature measuring device was fixed to the multitubular reactor 1 generally used. 本発明の計測器固定装置の一実施形態例と、それを用いて反応管内に温度計測器を固定した様子を示した側断面図である。It is the sectional side view which showed one embodiment of the measuring device fixing device of this invention, and the mode that the temperature measuring device was fixed in the reaction tube using it. 図2の管板5a側を拡大した図である。It is the figure which expanded the tube sheet 5a side of FIG. 図1に示す多管式反応器1の、管板5b側から見た断面図である。It is sectional drawing seen from the tube sheet 5b side of the multitubular reactor 1 shown in FIG. 本発明の計測器固定装置の他の実施形態例と、それを用いて反応管内に温度計測器を固定した様子を示した側断面図である。It is the sectional side view which showed a mode that the temperature measuring device was fixed in the reaction tube using another embodiment of the measuring device fixing device of this invention.

符号の説明Explanation of symbols

1 多管式反応器
6 反応管
10 温度計測器
20 計測器固定装置
21、22 糸条
21a 糸条の自由端
24 管状部材
25 固定部材
DESCRIPTION OF SYMBOLS 1 Multitubular reactor 6 Reaction tube 10 Temperature measuring device 20 Measuring device fixing device 21, 22 Yarn 21a Free end of yarn 24 Tubular member 25 Fixing member

Claims (4)

反応器が有する反応管内に計測器を固定し、触媒を充填する方法であって、
2本の糸条が取り付けられた計測器を、一方の糸条の一部が反応管の一方の開口よりも外側にあり、他方の糸条の一部が反応管の他方の開口よりも外側にあるように、反応管内に挿入し、
前記計測器が反応管の長さ方向の所定位置に位置するように、かつ反応管の内壁に接触しないように、2本の糸条を緊張させた状態で、反応管内に触媒を充填する、反応器への触媒の充填方法。
A method of fixing a measuring instrument in a reaction tube of a reactor and filling a catalyst,
A measuring instrument with two yarns attached, part of one yarn is outside one opening of the reaction tube, and part of the other yarn is outside the other opening of the reaction tube And insert it into the reaction tube,
The catalyst is filled in the reaction tube in a state where the two threads are tensioned so that the measuring instrument is located at a predetermined position in the length direction of the reaction tube and does not contact the inner wall of the reaction tube. A method for charging the catalyst into the reactor.
前記反応器が複数の反応管を有している多管式反応器であって、計測器を固定する装置を、計測器を固定する反応管とは別の反応管の開口部の形状を利用して固定する、請求項1に記載の反応器への触媒の充填方法。   The reactor is a multi-tubular reactor having a plurality of reaction tubes, and the device for fixing the measuring device uses the shape of the opening of the reaction tube different from the reaction tube for fixing the measuring device. The method for charging the catalyst into the reactor according to claim 1, wherein the catalyst is fixed. 反応器が有する反応管内に計測器を固定する装置であって、
前記計測器に取り付けられた2本の糸条のうち、一方の糸条の一部が反応管の一方の開口よりも外側にあるようにして、他方の糸条の一部を反応管の他方の開口よりも外側で、該糸条を緊張させた状態で固定する固定手段と、
前記計測器が前記反応管の内壁に接触しないように、固定手段で固定された前記糸条の位置を決める位置決め手段とを有する計測器固定装置。
A device for fixing a measuring instrument in a reaction tube of a reactor,
Of the two yarns attached to the measuring instrument, a part of one yarn is outside the one opening of the reaction tube, and a part of the other yarn is connected to the other of the reaction tube. Fixing means for fixing the yarn in a tensioned state outside the opening of
A measuring instrument fixing device comprising positioning means for determining a position of the yarn fixed by fixing means so that the measuring instrument does not contact the inner wall of the reaction tube.
前記反応器が複数の反応管を有している多管式反応器の反応管内に計測器を固定する装置であって、
前記位置決め手段が、計測器を固定する反応管とは別の反応管の開口部の形状を利用して固定し、前記固定手段で固定された糸条の位置を決める手段である、請求項3に記載の計測器固定装置。
An apparatus for fixing a measuring instrument in a reaction tube of a multi-tube reactor in which the reactor has a plurality of reaction tubes,
4. The positioning means is means for fixing using a shape of an opening of a reaction tube different from a reaction tube for fixing a measuring instrument, and determining a position of a yarn fixed by the fixing means. The measuring instrument fixing device described in 1.
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