JP2005325044A - 多管式反応器のパイロットテスト方法 - Google Patents
多管式反応器のパイロットテスト方法 Download PDFInfo
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- JP2005325044A JP2005325044A JP2004143307A JP2004143307A JP2005325044A JP 2005325044 A JP2005325044 A JP 2005325044A JP 2004143307 A JP2004143307 A JP 2004143307A JP 2004143307 A JP2004143307 A JP 2004143307A JP 2005325044 A JP2005325044 A JP 2005325044A
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- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
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- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
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- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8876—Arsenic, antimony or bismuth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
- B01J8/067—Heating or cooling the reactor
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/33—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/33—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties
- C07C45/34—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds
- C07C45/35—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds in propene or isobutene
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/215—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of saturated hydrocarbyl groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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Abstract
【解決手段】多管式反応器を構成する反応管と同様の反応管で、触媒層温度の測定手段が設けられた反応管少なくとも1本と、残余の測定手段が設けられていない反応管からなる複数本を熱媒体中に浸漬させ、それらの反応管に所定の原料ガスを流して反応させ、このときの触媒層の温度を測定すると共に、温度測定手段が設けられていない反応管では排出される反応生成ガスの反応結果を分析して、測定された触媒層温度での反応が、分析された反応結果をもたらすものとして多管式反応器の反応条件を設定するパイロットテスト方法及びその装置。
【選択図】なし
Description
次に、反応管aの反応転化率を98±0.3%に保つように熱媒体温度を調節しながら8ヶ月間運転を継続したところ、熱媒体温度は1.2℃上昇し、この間の合計収率は91.9%であった。
(1)上記多管式反応器に用いられる反応管と実質的に同一の反応管複数本を、温度調節可能な熱媒体中に浸漬させ、それら反応管は、触媒層温度を測定するための温度測定手段が設けられたもの少なくとも1本と、残余の温度測定手段が設けられていないものからなり、
(2)それら反応管に所定の原料ガスを所定量ずつ流し、熱媒体温度を調節して該原料ガスを反応管内の触媒層中で反応させて、
(3)温度測定手段が設けられた反応器では触媒層の温度を測定し、且つ
(4)温度測定手段が設けられていない反応管では排出される反応生成ガスの反応結果を分析して、
(5)(3)で測定された触媒層温度での反応が、(4)で分析された反応結果をもたらすものとして反応条件を設定する、
ことを特徴とするパイロットテスト方法及びそのための装置を提供するものである。
本発明は、多管式反応器を用いて気相接触反応を行う際の反応条件設定のためのパイロットテストの方法及びその装置に関するものである。
MoaWbBicFedAeDfEgGhJiOx (1)
MoaVbWcCudQeZfOx (2)
(1)触媒表面を解重合性を有する有機高分子化合物でコーティングして、触媒の機械的強度を向上させる方法(特公報2852712号公報)。
(2)触媒を反応管上部より落下充填するとき、反応管内に実質的に触媒の落下を妨げない形状及び太さを有するひも状物質を介在させる方法(特開平5−31351号公報)。
(3)触媒を落下充填するに先立って反応管内にドライアイスを充填し、次いで触媒を充填した後ドライアイスを気化させて除去する方法(特開平10−277381号公報)。
(4)触媒を落下充填するに先立って反応管内に液状物を充填し、次いで触媒を充填した後液状物を除去する方法(特開平9−141084号公報)。
(5)触媒充填時間を制御できる触媒供給コンベアを有する自動充填機を使用する方法(特開平11−333282号公報)。
などがあり、本発明における触媒の充填は、これらの方法の何れか又はこれらを適宜組み合わせて行うことができる。
触媒の調製
パラモリブデン酸アンモニウム94重量部を純水400重量部に加熱溶解させた。一方、硝酸第二鉄7.2重量部、硝酸コバルト25重量部及び硝酸ニッケル38重量部を純水60重量部に加熱溶解させた。これらの溶液を十分に攪拌しながら混合し、スラリー状の溶液を得た。
Mo12Bi5Ni3Co2Fe0.4Na0.2Mg0.4B0.2K0.1Si24Ox (3)
(但し、xはそれぞれの元素の酸化状態により定まる数値である。)
を有する固体粒子状のモリブデン−ビスマス系複合酸化物触媒を得た。
固体粒子状触媒を充填する前に反応管の上端から反応管底部に触媒押さえ表面までの長さを測定し、次いで触媒を充填した後、反応管の上端から触媒層表面までの長さを測定して、その差を触媒層の厚さとした。
標準反応条件時に多管式反応器に供給される原料ガス流量を、反応管の数で除すことによって各反応管に流れる原料ガスの平均流量を求め、この平均流量と同量の空気を検体の反応管に流してその差圧を測定した。すなわち、以下の実施例の多管式反応器による実機試験における標準反応条件時の原料ガス流量は12300Nm3/Hであるため、各反応管に流れる原料ガスの平均流量は1230NL/Hであった。
計測用反応管に、上記の反応管差圧の測定における非計測用反応管の差圧と同じ差圧をかけて空気を流したときに、該計測用反応管に流れる空気の量を測定した。
プロピレンの転化率、アクロレイン及びアクリル酸収率は以下の式に従って求めた。
非計測用反応管A1の作製
底部に触媒押さえを有する内径25.4mm、長さ3.5mのステンレス鋼製の管に、前記一般式(3)の固体粒子状の触媒物質に不活性物質として直径5mmのシリカ製ボールを混合して触媒活性を調節した固体粒子状触媒を使用し、反応管の反応原料ガス導入口から順に、触媒活性の比〔触媒物質量/(触媒物質量+不活性物質量)〕が0.5、0.7、1となるように、それぞれ順に350mL、340mL、790mLずつ充填して3層の触媒層を形成した。触媒層全体の厚さは300cmであり、この反応管A1に掛かる差圧は19kPaであった。
上記非測定用反応管A1と同様のステンレス鋼製の管に、振れ止め部材をつけた外径4mmの多点温度測定可能な熱電対(保護管内に熱電対が管軸方向に移動可能に挿入されたもの)を設置し、該反応管A1と同様、触媒活性を調節した固体粒子状触媒をそれぞれ315mL、306mL、711mLずつ充填してA1と同じ長さの触媒層を形成した。 触媒層全体の厚さは300cmであり、この反応管B1に掛かる差圧は20kPaであった。また反応管A1と同じ差圧を掛けて空気を流したときの流量は1170NL/Hであった。
パイロットテスト装置は、その装置の胴部(シェル)内に複数の反応管を保持する保持手段が設けられ、それら反応管の間を熱媒体が貫流する。熱媒体は加熱又は冷却可能な温度調節手段に接続されており、この熱媒体に浸漬した反応管を加熱又は冷却する。セットされた複数の反応管は、原料ガスを導入するため、それらの頂部にある原料ガス供給口がそれぞれガス流量調節手段を介して原料ガス供給手段に接続されている。原料ガス供給手段は反応管の原料ガス導入口のそれぞれに別々に、又は幾つかの反応管の導入口に一括して原料ガスを送ることができるような複数の手段を着脱可能に有している。反応管の反応生成ガス排出口はそれぞれ別々に、又は幾つかを一括して反応生成ガス分析手段に接続できる選択的な接続手段を有しており、計測用反応管の反応生成ガスは単独で、非計測用反応管の反応生成ガスは一括して、それぞれ別に反応生成ガス分析手段に接続される。さらに各反応管は、それぞれの触媒層にかかる差圧を測定するための手段にせつぞくされている。
非計測用反応管A1
プロピレン転化率:98.5モル%
アクロレイン収率とアクリル酸収率との合計:91.7モル%
計測用反応管B1
プロピレン転化率:98モル%
アクロレイン収率とアクリル酸収率との合計:92モル%
非計測用反応管A1
プロピレン転化率:97.5モル%
アクロレイン収率とアクリル酸収率との合計:90.3モル%
計測用反応管B1
プロピレン転化率:97モル%
アクロレイン収率とアクリル酸収率との合計:90.6モル%
多管式反応器は反応管10,000本組み込み可能な反応器シェル(内径4,500mm)を用い、パイロットテストに用いたものと同様の非計測反応管A1 9995本及び計測反応管B1 5本を組み込んだ。
プロピレン転化率:98.5モル%
アクロレイン収率とアクリル酸収率との合計:91.8モル%
プロピレン転化率:97.5モル%
アクロレイン収率とアクリル酸収率との合計:90.4モル%
非計測用反応管A2の作製
実施例1における非計測用反応管A1とほぼ同様にして3層の触媒層を形成した。
実施例1における計測用反応管B1とほぼ同様にして3層の触媒層を形成した。但し、外径32mmの多点温度測定可能な熱電対を用いる代わりに外径0.6mmの一点温度測定用熱電対を用いた。従って、A2とほぼ同じとなった。触媒層全体の厚さは300cmであり、この反応管B2に掛かる差圧は19kPaであった。
パイロットテスト装置による試験
非計測用反応管A2
プロピレン転化率:98.5モル%
アクロレイン収率とアクリル酸収率との合計:91.7モル%
計測用反応管B2
プロピレン転化率:98.5モル%
アクロレイン収率とアクリル酸収率との合計:91.7モル%
非計測用反応管A2
プロピレン転化率:97.5モル%
アクロレイン収率とアクリル酸収率との合計:90.3モル%
計測用反応管B2
プロピレン転化率:97.5モル%
アクロレイン収率とアクリル酸収率との合計:90.3モル%
実施例1において、非計測用反応管A1 9995本及び計測用反応管B1 5本を用いる代わりに、非計測反応管A2 9998本及び計測反応管B2 2本を用いる以外は実施例1とほぼ同様にして多管式反応器による実機試験を行った。原料ガスはゲージ圧130kPa(kPaG)、供給量12300Nm3/Hで供給された。熱媒体入口温度が330℃になるように設定した。触媒層の最高ピーク温度の平均は396℃であった。
プロピレン転化率:98.5モル%
アクロレイン収率とアクリル酸収率との合計:91.8モル%
プロピレン転化率:97.5モル%
アクロレイン収率とアクリル酸収率との合計:90.4モル%
Claims (9)
- 内部に固体粒子状触媒の層を有する多数の反応管により構成された多管式反応器を用いる気相接触反応の反応条件を設定するためのパイロットテスト方法であって:
(1)上記多管式反応器に用いられる反応管と実質的に同一の反応管複数本を、温度調節可能な熱媒体中に浸漬させ、それら反応管は、触媒層温度を測定するための温度測定手段が設けられた反応管少なくとも1本と、残余の温度測定手段が設けられていない反応管からなり、
(2)それら反応管に所定の原料ガスを所定量ずつ流し、熱媒体温度を調節して該原料ガスを反応管内の触媒層中で反応させて、
(3)温度測定手段が設けられた反応管では触媒層の温度を測定し、且つ
(4)温度測定手段が設けられていない反応管では排出される反応生成ガスの反応結果を分析して、
(5)(3)で測定された触媒層温度での反応が、(4)で分析された反応結果をもたらすものとして反応条件を設定する、
ことを特徴とするパイロットテスト方法。 - 酸化触媒がモリブデン−ビスマス系複合酸化物触媒又はモリブデン−バナジウム系複合酸化物触媒を含む請求項1に記載の方法。
- 温度測定手段が設けられた反応管及び温度測定手段が設けられていない反応管の触媒層が、実質的に同じ触媒層厚さを有する請求項1に記載の方法。
- 温度測定手段が設けられた反応管及び温度測定手段が設けられていない反応管に、実質的に同じ触媒層空間速度の原料ガスを流す請求項1に記載の方法。
- 反応結果が反応の目的物質の収率である請求項1に記載の方法。
- 請求項1〜5の何れかの方法に基づいて設定された反応条件に従って運転される多管式反応器によるプロパン、プロピレン又はイソブチレンの気相酸化方法。
- 内部に固体粒子状触媒の層を有する多数の反応管により構成された多管式反応器を用いる気相接触反応の反応条件を設定するためのパイロットテスト装置であって:
(1)上記多管式反応器に用いられる反応管と実質的に同一の反応管複数本が、共通の熱媒体中に浸漬され、それら反応管は、触媒層温度を測定するための温度測定手段が設けられたもの少なくとも1本と、残余の温度測定手段が設けられていないものからなり、熱媒体は加熱又は冷却可能な温度調節手段に接続されており、
(2)それら反応管は、その頂部にある原料ガス供給口がガス流量調節手段を介して原料ガス供給手段に接続され、
(3)温度測定手段が設けられた反応管底部の反応生成ガス排出口と、温度測定手段が設けられていない反応管底部の反応生成ガス排出口とは、それぞれ別々の反応生成ガス分析手段に接続され、且つ
(4)各反応管には、それぞれの触媒層にかかる差圧を測定するための手段を備えている、
ことを特徴とするパイロットテスト装置。 - 酸化触媒がモリブデン−ビスマス系複合酸化物触媒又はモリブデン−バナジウム系複合酸化物触媒を含む請求項7に記載の装置。
- 温度調節手段が熱交換器及び/又は加熱装置である請求項7に記載の装置。
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JP2004143307A JP2005325044A (ja) | 2004-05-13 | 2004-05-13 | 多管式反応器のパイロットテスト方法 |
CNB2004800005762A CN100425334C (zh) | 2004-05-13 | 2004-10-25 | 多管反应器的小规模试验方法 |
PCT/JP2004/016178 WO2005110591A1 (ja) | 2004-05-13 | 2004-10-25 | 多管式反応器のパイロットテスト方法 |
US11/596,293 US20080014127A1 (en) | 2004-05-13 | 2004-10-25 | Pilot test method for multitubular reactor |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2007268328A (ja) * | 2006-03-30 | 2007-10-18 | Sumitomo Chemical Co Ltd | 温度測定装置又はその保護管の設置方法 |
JP2009148757A (ja) * | 2007-12-20 | 2009-07-09 | Man Dwe Gmbh | チューブ束反応器 |
JP7316482B1 (ja) * | 2022-02-18 | 2023-07-27 | 日本化薬株式会社 | 多管式反応器の運転またはその準備行為をサポートする方法および装置 |
WO2023157699A1 (ja) * | 2022-02-18 | 2023-08-24 | 日本化薬株式会社 | 多管式反応器の運転またはその準備行為をサポートする方法および装置 |
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CN101274252A (zh) * | 2006-12-29 | 2008-10-01 | 亚申科技研发中心(上海)有限公司 | 一种催化工艺的开发装置及方法 |
WO2008080357A1 (en) * | 2006-12-29 | 2008-07-10 | Accelergy Shanghai R & D Center Co., Ltd. | High throughput catalytic process mass transfer investigation method |
DE102010006723A1 (de) | 2010-02-03 | 2011-08-04 | Süd-Chemie AG, 80333 | Reaktorvorrichtung und Verfahren zur Optimierung der Messung des Temperaturverlaufs in Reaktorrohren |
US11346826B2 (en) | 2019-09-30 | 2022-05-31 | Saudi Arabian Oil Company | System and apparatus for testing and/or evaluating an industrial catalyst |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH06296854A (ja) * | 1993-04-13 | 1994-10-25 | Hitachi Ltd | 反応器およびその製造方法 |
JPH10309457A (ja) * | 1997-04-23 | 1998-11-24 | Basf Ag | 反応装置及び流動材料の処理方法 |
JP2000185227A (ja) * | 1998-12-24 | 2000-07-04 | Mitsubishi Chemicals Corp | 高圧固定床反応器 |
JP2003001094A (ja) * | 2001-06-26 | 2003-01-07 | Nippon Shokubai Co Ltd | 固体粒子充填反応器およびその反応器を用いた接触気相酸化方法 |
JP2003206244A (ja) * | 2002-01-11 | 2003-07-22 | Mitsubishi Chemicals Corp | 気相接触酸化方法 |
Family Cites Families (1)
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JP2008031094A (ja) * | 2006-07-28 | 2008-02-14 | Kao Corp | Scf結合阻害剤 |
-
2004
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- 2004-10-25 WO PCT/JP2004/016178 patent/WO2005110591A1/ja active Application Filing
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH06296854A (ja) * | 1993-04-13 | 1994-10-25 | Hitachi Ltd | 反応器およびその製造方法 |
JPH10309457A (ja) * | 1997-04-23 | 1998-11-24 | Basf Ag | 反応装置及び流動材料の処理方法 |
JP2000185227A (ja) * | 1998-12-24 | 2000-07-04 | Mitsubishi Chemicals Corp | 高圧固定床反応器 |
JP2003001094A (ja) * | 2001-06-26 | 2003-01-07 | Nippon Shokubai Co Ltd | 固体粒子充填反応器およびその反応器を用いた接触気相酸化方法 |
JP2003206244A (ja) * | 2002-01-11 | 2003-07-22 | Mitsubishi Chemicals Corp | 気相接触酸化方法 |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2007268328A (ja) * | 2006-03-30 | 2007-10-18 | Sumitomo Chemical Co Ltd | 温度測定装置又はその保護管の設置方法 |
JP4582039B2 (ja) * | 2006-03-30 | 2010-11-17 | 住友化学株式会社 | 温度測定装置又はその保護管の設置方法 |
JP2009148757A (ja) * | 2007-12-20 | 2009-07-09 | Man Dwe Gmbh | チューブ束反応器 |
JP7316482B1 (ja) * | 2022-02-18 | 2023-07-27 | 日本化薬株式会社 | 多管式反応器の運転またはその準備行為をサポートする方法および装置 |
WO2023157699A1 (ja) * | 2022-02-18 | 2023-08-24 | 日本化薬株式会社 | 多管式反応器の運転またはその準備行為をサポートする方法および装置 |
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US20080014127A1 (en) | 2008-01-17 |
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