TW200528191A - Monitoring, control and/or regulation of reactions of a fluid reaction mixture in a reactor having thermoplates - Google Patents

Monitoring, control and/or regulation of reactions of a fluid reaction mixture in a reactor having thermoplates Download PDF

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Publication number
TW200528191A
TW200528191A TW93138975A TW93138975A TW200528191A TW 200528191 A TW200528191 A TW 200528191A TW 93138975 A TW93138975 A TW 93138975A TW 93138975 A TW93138975 A TW 93138975A TW 200528191 A TW200528191 A TW 200528191A
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TW
Taiwan
Prior art keywords
sleeve
reactor
gap
reaction mixture
sampling tube
Prior art date
Application number
TW93138975A
Other languages
Chinese (zh)
Other versions
TWI376267B (en
Inventor
Gerhard Olbert
Claus Hechler
Dietmar Loewen
Original Assignee
Basf Ag
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Publication date
Application filed by Basf Ag filed Critical Basf Ag
Publication of TW200528191A publication Critical patent/TW200528191A/en
Application granted granted Critical
Publication of TWI376267B publication Critical patent/TWI376267B/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02Chemical 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
    • B01J8/0285Heating or cooling the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/248Reactors comprising multiple separated flow channels
    • B01J19/249Plate-type reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/001Controlling catalytic processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00026Controlling or regulating the heat exchange system
    • B01J2208/00035Controlling or regulating the heat exchange system involving measured parameters
    • B01J2208/00044Temperature measurement
    • B01J2208/00061Temperature measurement of the reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00106Controlling the temperature by indirect heat exchange
    • B01J2208/00115Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
    • B01J2208/0015Plates; Cylinders
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00628Controlling the composition of the reactive mixture
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796Details of the reactor or of the particulate material
    • B01J2208/00946Features relating to the reactants or products
    • B01J2208/00955Sampling of the particulate material, the reactants or the products
    • B01J2208/00964Reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796Details of the reactor or of the particulate material
    • B01J2208/00946Features relating to the reactants or products
    • B01J2208/00955Sampling of the particulate material, the reactants or the products
    • B01J2208/00973Products
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00054Controlling or regulating the heat exchange system
    • B01J2219/00056Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058Temperature measurement
    • B01J2219/00063Temperature measurement of the reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00193Sensing a parameter
    • B01J2219/00195Sensing a parameter of the reaction system
    • B01J2219/002Sensing a parameter of the reaction system inside the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24Stationary reactors without moving elements inside
    • B01J2219/2401Reactors comprising multiple separate flow channels
    • B01J2219/245Plate-type reactors
    • B01J2219/2451Geometry of the reactor
    • B01J2219/2453Plates arranged in parallel
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24Stationary reactors without moving elements inside
    • B01J2219/2401Reactors comprising multiple separate flow channels
    • B01J2219/245Plate-type reactors
    • B01J2219/2461Heat exchange aspects
    • B01J2219/2462Heat exchange aspects the reactants being in indirect heat exchange with a non reacting heat exchange medium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24Stationary reactors without moving elements inside
    • B01J2219/2401Reactors comprising multiple separate flow channels
    • B01J2219/245Plate-type reactors
    • B01J2219/2476Construction materials
    • B01J2219/2477Construction materials of the catalysts
    • B01J2219/2481Catalysts in granular from between plates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24Stationary reactors without moving elements inside
    • B01J2219/2401Reactors comprising multiple separate flow channels
    • B01J2219/245Plate-type reactors
    • B01J2219/2476Construction materials
    • B01J2219/2483Construction materials of the plates
    • B01J2219/2485Metals or alloys
    • B01J2219/2486Steel
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24Stationary reactors without moving elements inside
    • B01J2219/2401Reactors comprising multiple separate flow channels
    • B01J2219/245Plate-type reactors
    • B01J2219/2491Other constructional details
    • B01J2219/2497Size aspects, i.e. concrete sizes are being mentioned in the classified document

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

A process is proposed for monitoring, controlling and/or regulating reactions of a fluid reaction mixture in the presence of a heterogeneous particulate catalyst, in a reactor having two or more thermoplates (1) arranged vertically and parallel to each other while in each case leaving a gap (2), the heterogeneous particulate catalyst being installed in the gaps (2) and the fluid reaction mixture being passed through the gaps (2), which comprises selecting as a regulation signal the temperature which is determined in one or more gaps (2), at two or more measurement points which are distributed over the height of each gap (2).

Description

200528191 九、發明說明: 【發明所屬之技術領域】 本發明係關於一種用於監視、控制及/或調節具有熱板之 反應裔内之流體反應混合物之反應之方法,且本發明亦γ夺 關於一種用於進行該方法之設備。 【先前技術】 在化學處理技術中,流體(意即,氣體、液體或氣體/液體 反應混合物)之許多反應(尤其亦係部分氧化反應)是已知 的,該等反應係在異質微粒催化劑存在之情況下進行的。 該等反應通常為放熱的,經常為強烈地放熱。其迄今已主 要在具有催化劑管之管束反應器内以工業規模進行,將異 質微粒催化劑引入至該等催化劑管中,且使流體反應混合 物通過該等催化劑管,且反應之所釋放之熱量係經由在催 化劑官間之中間空間内循環之熱載體來間接移除。所用之 熱載體經常為鹽熔體。 作為-替代,亦可經由通過板型熱轉移器之熱載體來移 除反應之熱!。術語熱交換器板、熱轉移器板及熱板大體 上同義地用於板型熱轉移器。 將熱轉移器板主要界定成具有一内部之薄片狀結構,該 ^具有人π及出口管線’且與表面區域相比具有較薄之 厚,。該等熱轉移器板通常係由金屬薄片製造,經常係由 薄片衣k ,然1^ ’視應用情況而S,特別係視反應介質 及熱載體之特性而定,可使用特定之、特別係抗腐蝕之、 或經塗佈之材料。用於熱載體之人口及出Π裝置通常排列 97923.doc 200528191 於熱交換器板之相對端處。所用之熱載體經常為水或 Diphyl (以重里# 70至75%之一苯醚與以重量計25至30%之 聯苯的混合物),該等熱載體有時亦會在煮沸作__ operation)中蒸發;亦可使用具有低蒸汽壓力之其它有機熱 載體亦及離子性液體。 用作熱載體之離子性液體的用途描述於德國專利申請案 DE-A 103 16 418中。優先選擇含有硫酸鹽、磷酸鹽、硼酸 鹽或矽酸鹽陰離子之離子性液體。含有單價金屬陽離子(特 別為鹼金屬陽離子)亦及另一陽離子(特別為咪唑鑌陽離子) 之離子性液體亦特別適合。含有作為陽離子之咪唑鑌、吡 °定鑌或鳞陽離子之離子性液體亦是有利的。 術語熱板特別係用於熱轉移器板,其單個(通常為兩個) 金屬薄片係藉由點焊及/或卷焊(r〇ll weld)而接合在一起, 且經常使用水壓將薄片塑性地成形以形成凹穴。 在本文中’在上文定義之意義上使用術語熱交換器板、 熱轉移器板及熱板。 用於使用熱板進行部分氧化之反應器係(例如)自DE-a 199 52 964中得知。該申請案描述了用於在反應器内在熱轉 移器板周圍的床上進行部分氧化之催化劑的排列。將反應 /匕a物於一反應為端處饋入至熱轉移器板間之反應器内部 並將其在相對端處移除,且其因此流過熱轉移器板間之中 間空間。 DE-C 197 54 185描述了另一反應器,其經由流過熱轉移 器板之冷卻介質間接地移除熱量,將該等熱轉移器板設計 97923.doc 200528191 成由至少兩鋼板組成之熱板,該等鋼板係於預定點處接合 在一起以形成流動通道。 其有利的開發係描述於DE-A 198 48 208中,根據該申請 案,將組態成冷卻介質流過之熱板的熱轉移器板組合成具 有(例如)矩形或正方形截面之板組件,且該等板組件具有外 殼。包裝板組件無需在圓周側上適應,且因此可以至圓柱 形反應裔容器之内壁的預定間距來使用。在外殼之上部區 域及下部區域内用導向板覆蓋板熱轉移器或其外殼與容器 内壁之間的自由表面,以防止反應介質繞過填充有催化劑 之腔室。 具有以板熱轉移器形式之用於移除反應之熱量之裝置的 另一反應器係描述於WO_A 01/8533 1 t。主要為圓柱形狀之 反應器含有一連續的催化劑床,該床中嵌入有板熱轉移器。 DE-A 103 33 866揭示了對作為變形之結果而出現之問題 亦及作為在高熱應力下再成形之結果之機械穩定性問題的 防止,其中该專變形係在反應混合物與外部環境之間存在 過高壓力差之情況下而在熱板之一側上存在高應力之結 果,當藉由提供一用於在異質微粒催化劑存在之情況下部 分氧化流體反應混合物之反應器使反應混合物處於高壓或 減壓下時,該等機械穩定性問題可能出現,該反應器具有: 或多個立方形熱板模組,其各由彼此平行排列、同時 在每一情況下均留有間隙之兩個或兩個以上矩形熱板形 成,該間隙可用異質微粒催化劑來填充,並使流體反應 混合物流過該間隙,反應之熱量係藉由流過該等熱板並 97923.doc 200528191 因此至少部分地蒸發之熱載體來吸收;該反應器具有: -一主要為圓柱形之外殼,該外殼在熱板模組處釋放壓力 並完全圍繞該等模組,且包括圓筒夾套及蓋(hood),其 在兩個末端處封閉該外殼,且其縱軸對準成平行於熱板 之平面;且該反應器亦具有: -一或多個密封元件,其以流體反應混合物除了流過由該 等蓋所界限之反應器内部空間外僅流過該等間隙之方式 排列。 【發明内容】 因此,本發明之一目的係提供一用於監視、控制及/或調 節反應器内進行之流體反應混合物之反應之方法,該反應 器具有安置於其内之熱板,異質微粒催化劑安置於該等熱 板間之間隙内且由反應介質所流過,且熱載體流過該等熱 板0 “因此,吾人已發現一用於監視、控制及/或調節在異質微 粒催化劑存在之情況下反應器内4流體反應混合物之反應 之方法’該反應器具有垂直且彼此平行排列、同時在每一 情況下均留有間隙之兩個或兩個以上熱板,異質微粒催化 劑安置於間隙内’且流體反應混合物通過該等間隙,該方 法包括選擇—或多個溫度作為—監視、控制及/或調節參 數’該或該等溫度係在—或多個間隙内於分佈在每—間隙 之高度上的一或多個量測點處得以量測。 ” 根據本务明’所4擇之監視、控制及/或調節參數為一或 多個溫度’該或該等溫度係在一或多個間隙内於分佈在每 97923.doc 200528191 -間隙之鬲度上的—或多個量測點處得以量測。 優先選擇係額外選擇一或多個間隙 之組份作為另一龄視、抻剎机體反應混合物 皿視、控制及/或調節參數,其 母間隙之尚度上的-或多個量測點處得以判定?刀 對於反應器之運行條件之判定,催化劑床中之 1°=^,及溫度之局部分佈‘:度 八佈對於反廍之里值與位置。沿反應介質之流動路徑的溫度 刀佈對於反應糸統之控似調節而言亦可能很重要。 除穩態運行外,亦必須控制啟動或停止或(例如)甚 過延長時期仍會隨_而變化之運行㈣界條件,例如, 催化劑活性(減活)之變化。基於量測溫度,可能(例如)確保 安全運行’而且可能控制並維持每一情況下均較佳之最優 運行狀態。可得出(例如)關於反應物組份與反應物流動速率 以及冷卻溫度與冷卻介質通過量(thr〇ughput)之最佳運行模 式的結論。此外,催化劑床中之額外濃度量測允許監視反 應之物質分佈,且(例如)亦允許在運行條件下判定反應動力 學(reaction kinetics)。舉例而言,亦可根據流通過程中之濃 度分佈、尤其連同溫度分佈一起使催化劑之減活行為特徵 化,其亦可藉由適應於反應物負載及處理流動速率而用於 具有低副產物形成之有利的反應控制,或用於催化劑及反 應器設計之改良。 發明者已認識到,可在量測運行本身不干擾該方法之情 況下判定已被引入至兩個熱板間之間隙内之微粒催化劑十 之在其高度上的溫度分佈(意即,沿流動路徑之溫度分佈)、 97923.doc -10- 200528191 亦及在催化劑之高度上之濃度分佈(意即,沿該流動路徑之 濃度分佈)。 對於可藉由根據本發明之方法來監視、控制及/或調節流 體反應混合物在異質微粒催化劑存在之情況下之化學反 應,原則上無限制。該等反應較佳為氣體反應混合物之反 應’尤其為氧化或部分氧化反應。 具有熱板之反應器已於上文中得以描述。 熱板較佳係由無腐蝕材料製造,尤其係由(例如)具有材 料編號1.4541或1·4404、以爪或以偏、1 4539或14547 與1.43 01之不銹鋼製造,或由其它合金鋼製造。 用於此目的之金屬薄片之材料厚度可在丨與4毫米、與 3毫米之間或在2與2.5毫米之間選擇,或為2·5毫米。 一般而言,可將兩個矩形金屬薄片在其縱向及末端側處 接合以產生熱板,在該情況下,可能存在卷狀接縫或橫向 焊=接頭或此等兩者之組合,使得其中稍後安置有熱載體 之空間在所有側上被密封。將熱板之邊緣在縱向邊緣之橫 向卷狀接縫處或甚至在其内有利地移除,使得冷卻較差(若 完全)且#中通常亦已安置有催化劑之邊緣區域具有很低 的幾何膨脹。 金屬薄片係藉由分佈在矩形表面上之點焊而接合在一 起。亦可能存在藉由直的或彎曲的亦及圓形卷狀接縫而連 接之至少局部分連接。亦可能藉由額外卷狀接縫將熱載體 所流過之容積分成複數個獨立區域。 在熱板上排列焊接點之一可能性為以具3〇至8〇毫米或h 97923.doc 200528191 毫米之等距點分離度的列排列,雖然亦可能為4〇至6〇 毫米之分離度,且另一實施例具有45至5〇毫米以及46至料 毫米之分離度。通常’由於製造之結果,點分離度會變化 多達土1毫米,且在板之縱向方向上來看,緊鄰列之焊接點 各係以偏移半個焊接點分離度的方式㈣。板之縱向方向 上之點焊之列可以5至5 〇毫米或8至2 5毫米之分離度等距排 列’雖然亦可使用H)至20毫米以及12至14毫米之分離度。 此外,亦可存在適應於應用情況之所提及之焊接點分離度 與列分離度的配對。列分離度可與點分離度成一定的幾何 關係’通常為點分離度之V4或稍微更低,使得在製造過程 中熱板有-定的均勾膨脹。對於預定之焊接點及列分離 度,指定每板表面積單位上之焊接點的一定數目;可能的 值為200至3000個焊接點/平方求板表面積,典型值為 至2600個焊接點/平方米板表面積。有利地,在5倍之焊接 點分離度乘5倍之列分離度之矩形表面截面上存在⑼至μ 個焊接點。熱板之寬度大體上受到製造技術考量之限制, 且該寬度可在100與2500毫米之間或在5〇〇與丨5〇〇毫米之 間。熱板之長度取決於反應,特別係取決於反應之溫度分 佈,且該長度可在500與7000毫米之間或在3〇〇〇與4〇〇〇毫米 之間。 Μ 在每一情況下,兩個或兩個以上熱板平行排列且彼此分 開以形成熱板模組。以此方式導致了形成於緊鄰板間之桿 狀間隙,該等熱板(例如)在板分離度之最窄點處具有在8與 150毫米之間或10至100毫米之寬度。一可能之實施例亦具 97923.doc -12- 200528191 有12至50宅米或14至25宅米之貧声雜妙__ 、見度雖然亦可選擇16至20 宅米之寬度。亦已測試了 17毫米之間隙分離度。200528191 IX. Description of the invention: [Technical field to which the invention belongs] The present invention relates to a method for monitoring, controlling and / or regulating the reaction of a fluid reaction mixture in a reaction line having a hot plate, and the present invention also relates to An apparatus for performing the method. [Prior art] In chemical processing technology, many reactions of fluids (that is, gas, liquid, or gas / liquid reaction mixtures), especially partial oxidation reactions, are known. These reactions exist in heterogeneous particulate catalysts. Carried out under circumstances. These reactions are usually exothermic, often intensely exothermic. So far, it has been mainly carried out on an industrial scale in a tube-bundle reactor with catalyst tubes, introducing a heterogeneous particulate catalyst into the catalyst tubes, and passing a fluid reaction mixture through the catalyst tubes, and the heat released by the reaction is via The heat carrier circulating in the intermediate space between the catalysts is removed indirectly. The heat carrier used is often a salt melt. As an alternative, the heat of reaction can also be removed via a heat carrier passing through a plate heat transfer! . The terms heat exchanger plate, heat transfer plate, and heat plate are used synonymously for plate-type heat transfer. The heat transfer plate is mainly defined as a sheet-like structure having an interior, which has a human π and an outlet pipeline 'and is thinner and thicker than the surface area. These heat transfer plates are usually made of metal foil, often made of thin film k, but 1 ^ 'depending on the application situation, especially depending on the characteristics of the reaction medium and the heat carrier. Specific, special systems can be used Corrosion resistant or coated material. The population and outlet devices for heat carriers are usually arranged at 97923.doc 200528191 at the opposite end of the heat exchanger plate. The heat carrier used is often water or Diphyl (a mixture of 70 to 75% by weight of phenyl ether and 25 to 30% by weight of biphenyl). These heat carriers are sometimes boiled for __ operation ); Other organic heat carriers with low vapor pressure and ionic liquids can also be used. The use of ionic liquids as heat carriers is described in German patent application DE-A 103 16 418. Preference is given to ionic liquids containing sulfate, phosphate, borate or silicate anions. Ionic liquids containing monovalent metal cations (especially alkali metal cations) and another cation (especially imidazolium cations) are also particularly suitable. Ionic liquids containing imidazolium, pyridine, or scale cations as cations are also advantageous. The term hot plate is used especially for heat transfer plates, whose single (usually two) metal sheets are joined together by spot welding and / or roll welding, and the sheets are often pressed using water pressure Plastically shaped to form a cavity. In this context, the terms heat exchanger plate, heat transfer plate and heat plate are used in the sense defined above. Reactors for partial oxidation using hot plates are known, for example, from DE-a 199 52 964. This application describes an arrangement of catalysts for partial oxidation in a reactor on a bed around a heat transfer plate. The reaction material is fed into the interior of the reactor between the heat transfer plates at one reaction end and removed at the opposite end, and it therefore flows through the intermediate space between the heat transfer plates. DE-C 197 54 185 describes another reactor which removes heat indirectly via a cooling medium flowing through a heat transfer plate. The heat transfer plate is designed 97923.doc 200528191 into a hot plate consisting of at least two steel plates. These steel plates are joined together at predetermined points to form a flow channel. Its advantageous development is described in DE-A 198 48 208, according to which the heat transfer plate configured as a heat plate through which a cooling medium flows is combined into a plate assembly having, for example, a rectangular or square cross section, And the board components have a housing. The packaging plate assembly need not be adapted on the circumferential side, and therefore can be used at a predetermined distance from the inner wall of the cylindrical reaction container. Cover the plate heat transfer unit or its free surface between the housing and the inner wall of the container with guide plates in the upper and lower areas of the housing to prevent the reaction medium from bypassing the chamber filled with the catalyst. Another reactor with means for removing the heat of the reaction in the form of a plate heat transfer is described in WO_A 01/8533 1 t. The predominantly cylindrical reactor contains a continuous catalyst bed in which a plate heat transfer device is embedded. DE-A 103 33 866 reveals the prevention of problems that arise as a result of deformation and also mechanical stability problems as a result of reforming under high thermal stress, where the special deformation is present between the reaction mixture and the external environment As a result of high stress on one side of the hot plate in the case of excessively high pressure differences, the reaction mixture is kept at a high pressure or by providing a reactor for partially oxidizing the fluid reaction mixture in the presence of a heterogeneous particulate catalyst Under reduced pressure, these problems of mechanical stability may occur. The reactor has: or a plurality of cuboidal hot plate modules, each of which is arranged in parallel with each other while leaving a gap in each case. Two or more rectangular hot plates are formed, and the gap can be filled with a heterogeneous particulate catalyst, and the fluid reaction mixture flows through the gap. The heat of the reaction is caused by flowing through the hot plates and at least partially evaporates. The heat carrier absorbs it; the reactor has:-a predominantly cylindrical shell which releases pressure at the hot plate module and completely surrounds the A module, which includes a cylindrical jacket and a hood, which closes the shell at two ends, and whose longitudinal axis is aligned parallel to the plane of the hot plate; and the reactor also has:-one or more A sealing element is arranged in such a way that the fluid reaction mixture only flows through the gaps except through the interior space of the reactor bounded by the covers. SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a method for monitoring, controlling, and / or regulating a reaction of a fluid reaction mixture in a reactor having a hot plate and heterogeneous particles disposed therein. The catalyst is placed in the gap between the hot plates and is flowed by the reaction medium, and the heat carrier flows through the hot plates. "Hence, we have found a mechanism for monitoring, controlling and / or regulating the Method for the reaction of 4 fluid reaction mixtures in the reactor in the case of 'the reactor has two or more hot plates arranged vertically and parallel to each other while leaving a gap in each case, heterogeneous particulate catalyst is placed on Within the gaps' and the fluid reaction mixture passes through the gaps, the method includes selecting—or multiple temperatures as—monitoring, controlling, and / or adjusting parameters that the or temperatures are distributed within—or across the gaps— It can be measured at one or more measurement points on the height of the gap. "The monitoring, control and / or adjustment parameter selected according to this matter is one or more temperatures. The temperature coefficient or those within one or more gaps in the distribution of each 97923.doc 200528191 - of the gap of the Ge - measuring point to measuring the amount or more. Preferential selection refers to the additional selection of one or more gap components as another age vision, the brake body reaction mixture, the control, and / or adjustment parameters of the parent gap, or the number of measurement points Was it judged? Knife For the determination of the operating conditions of the reactor, 1 ° = ^ in the catalyst bed, and the local distribution of temperature, ‘: Degrees and locations of the opposite values in the cloth. The temperature along the flow path of the reaction medium may also be important for the control of the reaction system. In addition to steady-state operation, operating boundary conditions, such as changes in catalyst activity (deactivation), must also be controlled to start or stop or, for example, continue to change over extended periods of time. Based on the measured temperature, it is possible (for example) to ensure safe operation 'and it is possible to control and maintain the optimal optimal operating conditions in each case. Conclusions can be drawn, for example, on the optimal operating mode of the reactant components and reactant flow rate, as well as the cooling temperature and the cooling medium throughput (throughput). In addition, additional concentration measurements in the catalyst bed allow monitoring of the material distribution of the reaction and, for example, also allow determination of reaction kinetics under operating conditions. For example, the deactivation behavior of the catalyst can also be characterized based on the concentration distribution in the flow-through process, especially in conjunction with the temperature distribution, which can also be used to have low by-product formation by adapting to reactant loading and processing flow rates. The favorable reaction control, or the improvement of catalyst and reactor design. The inventors have recognized that it is possible to determine the temperature distribution (i.e., along the flow) of the particulate catalyst that has been introduced into the gap between two hot plates without the measurement operation itself interfering with the method. The temperature distribution of the path), 97923.doc -10- 200528191 and the concentration distribution at the height of the catalyst (that is, the concentration distribution along the flow path). There are in principle no restrictions on the chemical reaction of the fluid reaction mixture in the presence of heterogeneous particulate catalysts that can be monitored, controlled and / or adjusted by the method according to the invention. These reactions are preferably reactions of gaseous reaction mixtures, especially oxidation or partial oxidation reactions. Reactors with hot plates have been described above. The hot plate is preferably made of a non-corrosive material, in particular stainless steel with material number 1.4541 or 1.4404, claw or bias, 1 4539 or 14547 and 1.43 01, or other alloy steel. The material thickness of the metal foil used for this purpose can be selected between 丨 and 4 mm, and 3 mm, or between 2 and 2.5 mm, or 2.5 mm. In general, two rectangular metal foils can be joined at their longitudinal and end sides to produce a hot plate, in which case there may be rolled seams or transverse welds = joints or a combination of both, such that The space where the heat carrier is placed later is sealed on all sides. The edge of the hot plate is advantageously removed at or in the transversely rolled seam of the longitudinal edge, so that the cooling is poor (if complete) and the edge area where the catalyst is usually also placed has a low geometric expansion . The metal foils are joined together by spot welding distributed over a rectangular surface. There may also be at least partial connections that are connected by straight or curved and round rolled seams. It is also possible to divide the volume through which the heat carrier flows into a plurality of separate areas by means of additional roll-up seams. One possibility of arranging the solder joints on the hot plate is to arrange in rows with equidistant dot separations of 30 to 80 mm or h 97923.doc 200528191 mm, although separations of 40 to 60 mm may also be possible And another embodiment has a resolution of 45 to 50 millimeters and 46 to 50 millimeters. Normally, as a result of manufacturing, the point separation varies by as much as 1 mm, and in the longitudinal direction of the plate, the welding points in the next row are each offset by half the welding point separation. The spot-welding columns in the longitudinal direction of the plate can be equidistantly arranged with a separation of 5 to 50 mm or 8 to 25 mm ', although separations of 20 to 20 mm and 12 to 14 mm can also be used. In addition, there may be a pairing of the mentioned joint separation and row separation to suit the application. The column separation degree can have a certain geometric relationship with the point separation degree, which is usually V4 or slightly lower than the point separation degree, so that the hot plate has a constant uniform expansion during the manufacturing process. For the predetermined welding point and row separation, specify a certain number of welding points per unit of surface area of the plate; possible values are 200 to 3000 welding points / square. Find the surface area of the plate, typical values are up to 2600 welding points / square meter. Board surface area. Advantageously, there are ⑼ to μ welding points on a rectangular surface cross section of 5 times the welding point separation times 5 times the column separation. The width of the hot plate is generally limited by manufacturing technology considerations, and the width can be between 100 and 2500 mm or between 500 and 500 mm. The length of the hot plate depends on the reaction, especially the temperature distribution of the reaction, and the length can be between 500 and 7000 mm or between 3,000 and 4,000 mm. Μ In each case, two or more hot plates are arranged in parallel and separated from each other to form a hot plate module. This results in a rod-shaped gap formed immediately between the plates, which, for example, have a width between 8 and 150 mm or 10 to 100 mm at the narrowest point of plate separation. A possible embodiment is also 97923.doc -12- 200528191. There are 12 to 50 house meters or 14 to 25 house meters of poor sound. __, although the visibility can also choose the width of 16 to 20 house meters. Gap resolution of 17 mm has also been tested.

在熱板模組之個別熱板之間,例如在大表面積板之情況 下,可額外地安置多個間隔片,以防止可改變板分離度或 位置之變形。為安置該等間隔片,可(例如)藉由較大直徑之 圓形卷狀接縫或焊接點而自熱載體之流動區域移除金屬板 之截面’以(例如)能夠將截面中間之孔引入至用於桿形間隔 片之板中,該等間隔片可由螺絲或焊接物固定。 個別板間之間隙可具有相同的分離度,但(若需要)當反 應允终或所要之反應需要、或可達成設備或冷卻技術優點 時,該等間隙亦可具有不同的寬度。 熱板模組之以催化劑微粒填充之間隙可相對於彼此每 封,例如藉由焊接來密封’或在處理側上接合在一起。 為了在將個別熱板接合在-起以形成模組時調整所要之 «分離度’將該等板以於其位置中並以分離度固定。Between individual hot plates of the hot plate module, for example, in the case of a large surface area plate, a plurality of spacers may be additionally disposed to prevent deformation that can change the plate separation or position. To place these spacers, the cross section of the metal plate can be removed from the flow area of the heat carrier, for example, by a larger diameter circular rolled seam or weld, to enable, for example, the hole in the middle of the cross section. Introduced into plates for rod-shaped spacers, which can be fixed by screws or welding. The gaps between individual plates can have the same degree of separation, but (if needed) these gaps can also have different widths when the response is finally required or the desired reaction is required, or when equipment or cooling technology advantages can be achieved. The gaps filled with the catalyst particles of the hot plate module can be sealed relative to each other, for example, by welding 'or bonded together on the processing side. In order to adjust the desired «resolution" when joining individual hot plates together to form a module, the plates are placed in their positions and fixed with the resolution.

直接相鄰之熱板之焊接點可彼此相對或彼此偏移。 一本=明亦提供-用於進行上文所述之方法之設備其以 套冋為特徵’該套筒安置於兩個熱板間之間隙内,較佳 在縱向方向上,且在反應器外部打開並密封溫度量測插 件,例如具有—或多個量測點之一或多個熱元件。 熱板較佳安置於: 产〆们立方形熱板模組中,其各由彼此平行排列、同 在每^况下均留有間隙之兩個或兩個以上矩形熱板 形成, 97923.doc -13- 200528191 熱板模組完全由釋放壓力之主要為圓柱形的外殼所包 圍"亥外〃又包括圓筒夾套及蓋,其於兩個末端處封閉該 外殼,且其縱轴對準成平行於熱板之平面, --或多個密封元件以流體反應混合物除了流過由該等蓋 所界限之反應n内部外僅流過該等間隙之方式排列,及 -具有—或多個相互獨Α之溫度量測插件之每一熱板模組 較佳均配備有兩個或三個、更佳為三個溫度量測插件。 根據在每凊况下均配備有至少一獨立之溫度量測插件 =每-熱板模組’彳個別地評估並監視每—熱板模組。為 每一熱板杈組提供一個以上溫度量測插件係有利的,使得 j個別/皿度里測插件失效之情況下,仍能確保安全運行。 當在每一情況下每熱板模組上使用三個溫度量測插件時, 可能在溫度量測插件之測試、維護或失效之情況下、尤其 係當溫度訊號功能上用於保護電路中時維持安全運行。 套筒係一較佳金屬管,其尤其具有4至15毫米、特別為6 至10¾米、經常為6至8毫米範圍内之外徑,且其進一步較 佳具有0.8至1.5毫米、較佳為(毫米之壁厚度。雖然套筒及 熱板不必由相同的材料製成,但是可用於套筒之材料原則 係/、了用於熱板之材料相同的材料。亦可將非鐵材料用 作套筒。 根據先前技術,當將溫度量測套筒或溫度量測插件插入 於催化劑床中時,有必要在管束反應器之情況下使用具有 增加之内徑之特別製造的管,以使反應分佈能夠等同於此 等官中之剩餘正常反應管中之反應分佈,且因此等同於代 97923.doc -14- 200528191 表性温度量測。 θ雖然與無安置套筒之反應管相比,用於容納反應管内之 量測元件之套筒中心地在其縱軸上之常見排列導致流動及 溫度分佈高度失真’且因此需要反應管、催化劑裝料亦及 (例如)在截面上具有不同壁厚度之套筒的特定組態或套筒 在催化劑管内之特定排列,如DE_Al〇l 1〇 847中所描述, 但是已發現’令人驚奇地,具有熱板之反應器未必需要熱 板間之間隙内之4等特定排列來量測催化劑床内之溫度分 佈0 从僅需要將溫度量測插件本身或密封該溫度量測插件之套 筒安置於間隙内,較佳將其安置於兩個熱板間之縱向方向 上。 /凰度里測插件或套筒與兩個熱板之距離在每一情況下較 仏可相等’意即’在一實施例中,溫度量測插件中心地安 置於間隙内。 為了將套筒引入至熱板間之間隙内,當熱板各具有相同 的焊接點圖案且相鄰熱板之焊接點相互相對時係特別有利 的。 套筒可在反應為外部在其上與其下打開。在一較佳實施 例中’套同可在反應器上與在其下打開。在該情況下,可 使μ度里測插件在套筒内連續地移位,使得不僅可判定離 政μ度S測’而且還可判定溫度分佈之連續說明。為此目 的可使用個別量測元件,但亦可有利地使用特別有利地 八有等距里测分離度之多重量測元件,因為用於不間斷地 97923.doc -15- 200528191 1翁度分佈之必要移位路徑因而僅為—量測點分離度。 套同可被無縫地引導通過外部反應器套,或在裝載催化 劑之熱板模組上方的區域内或在自下部引人之情況下在熱 板模組下方的區域内具有連接元件。在一特別有利之變體 中,套筒在反應器内部具有斷開,點,該等斷開點被特別設 計成切斷環式連接或夾1切接,使得顯練㈣地製成 組件。The soldering points of directly adjacent hot plates can be opposite or offset from each other. A book = also provided-equipment for carrying out the method described above, which is characterized by a sleeve 'the sleeve is placed in the gap between the two hot plates, preferably in the longitudinal direction, and in the reactor The temperature measurement insert is opened and sealed externally, for example with one or more thermal elements with one or more measurement points. The hot plates are preferably placed in: Cube-shaped cubic hot plate modules, each of which is formed by two or more rectangular hot plates arranged in parallel to each other with a gap in each case, 97923.doc -13- 200528191 The hot plate module is completely surrounded by a predominantly cylindrical shell that releases pressure. "The outer shell also includes a cylindrical jacket and a cover, which closes the shell at both ends, and its longitudinal axis is opposite Quasi-parallel to the plane of the hot plate,-or the plurality of sealing elements are arranged in such a way that the fluid reaction mixture flows through the gaps except through the interior of the reaction bounded by the covers, and-has-or more Each hot plate module of each of the independent temperature measurement plug-ins is preferably equipped with two or three, more preferably three temperature measurement plug-ins. According to each condition, at least one independent temperature measurement plug-in is provided = each-hot-plate module ', each of which is individually evaluated and monitored. It is advantageous to provide more than one temperature measurement plug-in for each hot plate branch group, so that even if the individual plug-in / dip measurement plug-in fails, safe operation can still be ensured. When using three temperature measurement plugs on each hot plate module in each case, it may be in the case of testing, maintenance or failure of the temperature measurement plug, especially when the temperature signal function is used to protect the circuit Maintain safe operation. The sleeve is a preferred metal tube, which especially has an outer diameter in the range of 4 to 15 mm, especially 6 to 10 ¾ meters, often in the range of 6 to 8 mm, and further preferably has 0.8 to 1.5 mm, preferably (Millimeter wall thickness. Although the sleeve and the hot plate do not have to be made of the same material, the material principle applicable to the sleeve is the same material used for the hot plate. Non-ferrous materials can also be used According to the prior art, when a temperature measuring sleeve or a temperature measuring insert is inserted into a catalyst bed, it is necessary to use a specially manufactured tube having an increased inner diameter in the case of a tube bundle reactor in order to make the reaction The distribution can be equivalent to the reaction distribution in the remaining normal reaction tubes in these officials, and is therefore equivalent to the apparent temperature measurement of generation 97923.doc -14- 200528191. θ Although compared with a reaction tube without a sleeve, The common arrangement on the longitudinal axis of the sleeve centering the measuring element inside the reaction tube results in a highly distorted flow and temperature distribution 'and therefore requires a reaction tube, catalyst charge and, for example, different wall thicknesses in section Of The specific configuration of the sleeves or the specific arrangement of the sleeves within the catalyst tube, as described in DE_Al0l 10847, but it has been found that 'surprisingly, a reactor with hot plates does not necessarily require a gap between the hot plates 4th specific arrangement to measure the temperature distribution in the catalyst bed. 0 It is only necessary to place the temperature measurement insert itself or the sleeve sealing the temperature measurement insert in the gap, preferably it is placed between two hot plates. In the longitudinal direction. / The distance between the measuring plug or sleeve and the two hot plates in each case may be equal in each case. 'Meaning' In one embodiment, the temperature measuring plug is centrally placed in the gap. In order to introduce the sleeve into the gap between the hot plates, it is particularly advantageous when the hot plates each have the same pattern of welding points and the welding points of adjacent hot plates are opposed to each other. The sleeve can react on the outside on it Instead of opening below. In a preferred embodiment, the sleeve can be opened on and below the reactor. In this case, the μ-degree measuring insert can be continuously displaced in the sleeve, so that not only can be determined Departure μ degree S test 'and can also determine Continuous description of the temperature distribution. For this purpose individual measuring elements can be used, but it is also advantageous to use particularly advantageous multi-weight measuring elements for measuring the resolution in equidistance, as it is used for uninterrupted 97923.doc -15 -200528191 The necessary displacement path of the 1 degree distribution is therefore only-measurement point separation. The package can be guided seamlessly through the external reactor jacket, or in the area above the hot plate module containing the catalyst or in the In the case of being introduced from below, there are connecting elements in the area below the hot plate module. In a particularly advantageous variant, the sleeve has breaks, points inside the reactor, which break points are specially designed Cut off the ring connection or the clip 1 to make the assembly obviously.

溫度量測插件通常具有分佈在其長度上並因此分佈在間 隙之高度上的複數個量測點。雖然亦可使用諸㈣電阻溫 度計(例如PT_1G()或ΡΤ-则)、電阻溫度計或半導體感應器 之所有其它(尤其係物理的)溫度量測原理’但是有用的溫度 量測插件較佳為多重量測插件(稱作多重熱元件)。視使用之 溫度而定,有用的熱元件係描述於DIN43710&DIN EN 60584中之王部熱元件,較佳為根據〇爪60584之κ型熱 元件。 … 可將所分佈之量測點等距排列,但在具有預期溫度極限 及/或特別大的溫度梯度之反應器區域内以彼此間有相對 較小之分離度且在剩餘反應器區域内以彼此間有相對較大 之分離度來排列該等量測點係特別有利的。 溫度量測插件有利地具有5至6〇個量測點,較佳具有ι〇 至50個量測點,更佳具有15至4〇個量測點,且仍更佳具有 20至3 0個量測點。 在一較佳實施例中,溫度量測插件具有2〇個量測點及約 3.8毫米之外徑,使得該溫度量測插件可安置於一具有6毫 97923.doc -16- 200528191 米或1/4英吋之外徑及4毫米 /、次5/32央吋之内徑的套筒内。 在另一較佳實施例中,择旦、、日丨4 _ 風又里測插件具有40個量測點及 約2 · 5毫米之外徑,你怨士女 、 于该&度1測插件可安置於一具有5 毫米或咖英时之外徑及3毫米或ι/8英时之内徑的套筒内。 在只知例中,雄封熱元件之套筒可安置於兩個熱板間 =間隙之橫向邊界處。為防止量測失真,在該情況下優先 選擇係在間Ρϋ向邊界與套筒之間提供絕緣元件,使得 亦可在床之邊緣處獲得代表性溫度訊號。在該情況下,以 下做法係特別有利的:套筒以固定方式安置於間隙内並保 持在彼處且不必將4套筒連同催化劑裝料—起安置並移 除在。亥It況下,亦可將套筒設計成具有非圓柱形幾何形 狀,例如具有正方形或半圓形截面。 另外,,亦可將密封溫度量測插件之套筒水平地安置於兩 個熱板間之方式允許在間隙之截面上判定溫 度分佈。 在發明性設備之另一較佳實施例中,除上文所描述之具 有溫度量測插件之套筒外,在每—情況下,在—或多個間 隙内提供一套筒,且該套筒具有多個穿孔亦及用於引入至 套筒内部之至少一取樣管,該取樣管以如下方式安置於彼 處:流體反應混合物流過套筒中之穿孔而進入該取樣管内 部’且此後自該取樣管中將流體反應混合物移除至反應器 外部並對其加以分析。 所用之套筒通常為金屬管,其較佳具有5至15毫米、特別 為8至1〇毫米範圍内之外徑及較佳為1毫米之壁厚度。根據 97923.doc •17- 200528191 =發明’套筒具有朝著反應空間之多個穿孔(意即,孔),該 寺孔原則上關於其幾何形狀無限制。然而,優先選擇具有 α开/形狀之孔„羊3之,亦可能為狹槽排列在取樣管之縱 向方向上之狭槽形形狀。該等穿孔較佳具有套筒之總的央 套表面積之1至50〇/〇、較佳為n〇%的總表面積。其用於允 許流體反應混合物流進套筒内,並因此經由套筒之孔而進 入安置於套筒内部的取樣管中。在反應器外自取樣管所採 取之樣品可藉由(例如)可用的工廠分析儀器來加以分析。同 樣可能連續地或以特定時„隔來採取樣品並分析樣品。 樣品之取出可由反應系統之自生壓力來實現,該自生壓力 係,由控制閥或溢流裝置、或藉由栗或壓縮機或散熱器/喷 射器來產生’在該情況下’可將樣品引入至一具有大氣壓 力或相對於该大氣之減壓或高壓的系統中。優先選擇係以 I·互定C力來控制其中引入樣品之分析系統,以增加量測精 度0 在一較佳實施例中,穿孔的套筒中心地安置於間隙内。 在此排列中,在特別小的程度上破壞間隙内流動分佈之對 稱性。可自上部或底部垂直地安置,且較佳自反應器之與 流體反應混合物之饋入側相同之側安置。 在安置有套筒且在每一情況下流體反應混合物係自上部 饋入至反應器内的實施例中,套筒僅在間隙之上部區域 内、尤其高達其中點附近有利地配備有多個穿孔。由於取 樣官僅在套筒之上部區域内延伸高達為判定樣品組份之目 的而藉由孔採取该樣品處之點,所以安置於此點下方之套 97923.doc -18- 200528191 筒的工白區域將$外組成反應混合物之旁路。此係藉由僅 在間隙之上部區域内提供套筒中之多個穿孔而得以防止。 巧似地’可安置套筒並在每—情況下將流體反應混合物 自下饋人至反應器内’且可較佳使熱載體通過熱板並使 熱載體在反應條件下部分地或完全地煮沸。 取樣管可較佳以如下方式以固定方式連接至套筒:該取 樣管之孔直接安置於套筒之穿孔上,絲樣管與套筒之孔 因此重疊。 在另一較佳實施例中,取樣管以可旋轉方式安置於穿孔 的套筒内,且具有安置於其夾套表面上之以如下方式偏移 之至少兩個孔:流體反應混合物總是僅藉由該等孔中之一 孔流進取樣管中。取樣管之孔較佳作為狹槽而安置於其縱 向方向上,此使得當使套筒與取樣管之孔匹配時讓出更多 可用的機動空間。 该貫施例允許藉由單個取樣管自分佈在間隙之高度上的 複數個點採取樣品。 在另一較佳變體中,每一取樣管具有至少兩個、較佳為 兩至四個相互獨立之腔室,每一腔室均具有一孔,流體反 應混合物藉由套筒之穿孔而流進該孔中,且將該流體反應 混合物單獨自每一腔室移除並對其加以分析。該等腔^ 相互相鄰地或同心地排列。 取樣管内兩個或兩個以上獨立腔室之形成增加了量測點 之數目,在該等量測點處可採取流體反應混合物之樣品。 特佳之實施例係取樣管設有複數個腔室且其另以可旋轉 97923.doc -19- 200528191 方式環繞其縱軸設置。以此方式允許每一腔室之兩個或雨 個以上、較佳為四個相互偏移狹槽容納待安置之流體反應 混合物,在該情況下,流體反應混合物在每一情況下總是 僅藉由一孔而流進每一腔室中。該實施例進一步增加了用 於^體反應混合物之組份的量測點之數目。 在另一較佳實施例中,提供兩個或兩個以上取樣管,並 將該等取樣管各以如下方式以固定方式連接至套筒:每一 取樣管之孔係直接安置於套筒之穿孔上,且個別取樣管在 間隙内各於不同的高度處打開。此外,亦可藉由如下方法 將套筒本身組態成取樣管··僅在與一取樣管於每一情況下 均存在直接連接之點處提供穿孔,且額外地在套筒内於一 不同於取樣管之開口的點處提供單個另外穿孔,流體反應 混合物係藉由該穿孔而流入。 因此,根據本發明之方法及設備使得以簡單方式利用可 用之工廠分析儀器來得到實際反應事件及真實溫度(較佳 亦係對熱點至關重要的溫度)之精確知識變得可能。以此方 式允許大體上更接近於催化劑之負載極限的操作;因此可 更好地利用催化劑,且同時可防止由不良之高熱點形成所 產生之損害。另外,根據實際反應事件之知識,催化劑活 性可以匹配實際反應事件之變化方式而空間地組態在^隙 内。以此方式保護催化劑,尤其係在更多熱應力之區域内 之催化劑,且因此更好地調整其老化,以為了更長或更有 利的利用之目的。 另外,反應器可大體上更均勻地運作,此可對於其中發 97923.doc -20- 200528191 生之反應的總選擇性產生正面的影響。另外,催化劑活性 對實際反應事件之適應允許減少熱載體之所需量。 在下文將參考圖式來詳細說明本發明。 【貫施方式】 圖1顯示一具有熱板1與其中已引入固定催化劑床之中間 間隙2之反應裔之截面的圖解。在所示之較佳實施例中,套 筒3中心地安置於間隙2内,且密封(例如)具有4個量測點之 熱元件4。套筒3及熱元件4通過反應器套中之噴嘴而突出於 反應器外。 圖1A中之橫截面說明了具有安置於其中之熱元件4之套 筒3的圓柱形幾何形狀。 圖2中之圖解說明顯示在未圖示之兩個熱板間之間隙乂 區域内於縱向方向上之反應器的截面。在間隙2中,在其橫 向邊界6處安置一具有熱元件4之套筒3。在套筒3與間隙2 之橫向邊界之間提供絕緣元件5。 圖2中之検截面說明了熱板丨(包含其對橫向邊界6之固 定)、亦及具有熱元件4之㈣3的圓柱形設計與絕緣元件5 的形狀適合設計。 圖3顯示具有熱元件4之套筒3於間隙2内水平排列之另一 實施例之橫面的圖解。該套筒在其突出至間隙内之末端附 近具有穿孔7,可藉由該等穿孔來採取反應混合物之樣品。 圖4中之圖解說明顯示具有套筒3之另一實施例之縱向截 面,該套筒3具有在套筒3内之用以將樣品採取進取樣管8 中之穿孔7。具有取樣管8之套筒3超過噴嘴9而突出於該反 97923.doc 21 200528191 應器外。 圖4A中之檢截面說明在截面内說明具有孔7及取樣管8之 套筒3之實施例。 圖5顯示一具有平行熱板丨與中間間隙2之反應器之截面 的圖解。以實例說明之,套筒3被顯示且在其縱向方向上突 出至兩個熱板1間之間隙2内,且該套筒藉由反應器套内之 噴嘴9而在反應器外部打開。 圖6顯不熱板表面上之兩較佳焊接點分佈:在每一情況 下,其說明對應於水平軸線上之5倍的焊接點分離度與垂直 軸線上之5倍的列分離度之熱板丨之矩形表面截面。圖6中之 上部說明顯示一較佳焊接點分佈,其在具有5倍的焊接點分 離度與5倍的列分離度之熱板丨的所示之表面截面上具有總 共33個焊接點,且下部說明顯示另一較佳排列,其在相同 尺寸之表面截面上具有25個焊接點。 【圖式簡單說明】 圖1顯示一具有熱板之反應器的截面,該等熱板在縱向截 面内具有一用於容納熱元件之中心安置的套筒,圖1A中為 橫截面說明, 圖2顯示在縱向截面内具有橫向安置之套筒之另一實施 例的截面,圖2A中為橫截面說明, 圖3顯示在縱向截面内具有水平安置於間隙内之套筒的 另一實施例,圖3A中為橫截面說明且圖36中為詳細說明, 圖4顯示在縱向截面内具有一具有穿孔及取樣管之套筒 之另一實施例的截面,圖4 A中為橫截面說明, 97923.doc -22- 200528191 圖5顯示發明性套筒在熱板模組内之安置的圖解說明’且 圖6顯示熱板表面上之較佳焊接點分佈的圖解。 在該等圖中,相同的參考數字指示相同或相應的特徵。 【主要元件符號說明】 1 熱板 2 間隙 3 套筒 4 熱元件 5 絕緣元件 6 橫向邊界 7 穿孔 8 取樣管 9 喷嘴 97923.doc -23 -A temperature measurement insert usually has a plurality of measurement points distributed over its length and therefore over the height of the gap. Although various other resistance thermometers (such as PT_1G () or PT-then), resistance thermometers, or all other (especially physical) temperature measurement principles of semiconductor sensors can also be used, useful temperature measurement plug-ins are preferably multiple Measurement plug-in (called multiple thermal element). Depending on the temperature used, useful thermal elements are described in DIN43710 & DIN EN 60584 as king thermal elements, preferably kappa type thermal elements according to 0 jaw 60584. … The measurement points distributed can be arranged equidistantly, but within a region of the reactor with the expected temperature limit and / or a particularly large temperature gradient with a relatively small degree of separation from each other and within the remaining reactor area with It is particularly advantageous to arrange these measurement points with a relatively large degree of separation from each other. The temperature measuring plug-in advantageously has 5 to 60 measuring points, preferably has ι to 50 measuring points, more preferably has 15 to 40 measuring points, and still more preferably has 20 to 30 measuring points. Measure points. In a preferred embodiment, the temperature measurement plug-in has 20 measurement points and an outer diameter of about 3.8 mm, so that the temperature measurement plug-in can be placed at a distance of 6 mm 97923.doc -16- 200528191 meters or 1 / 4 inch outer diameter and 4 mm / second 5/32 inch inner diameter sleeve. In another preferred embodiment, the Zandan test module has 40 measurement points and an outer diameter of about 2.5 millimeters. The insert can be placed in a sleeve with an outer diameter of 5 mm or cain and an inner diameter of 3 mm or ι / 8 in. In the known example, the sleeve of the male-sealed thermal element can be placed at the lateral boundary between the two hot plates = the gap. In order to prevent measurement distortion, it is preferred in this case to provide an insulating element between the boundary between the P-direction and the sleeve, so that a representative temperature signal can also be obtained at the edge of the bed. In this case, it is particularly advantageous that the sleeve is placed in the gap in a fixed manner and held there without having to place and remove the 4 sleeve together with the catalyst charge. In this case, the sleeve can also be designed to have a non-cylindrical geometry, such as a square or semi-circular cross section. In addition, the method of horizontally placing the sleeve of the sealed temperature measuring insert between the two hot plates allows the temperature distribution to be determined on the cross section of the gap. In another preferred embodiment of the inventive device, in addition to the sleeve with a temperature measuring insert described above, in each case, a sleeve is provided in one or more gaps, and the sleeve The cartridge has a plurality of perforations and at least one sampling tube for introduction into the interior of the sleeve, the sampling tube being positioned there as follows: the fluid reaction mixture flows through the perforations in the sleeve and enters the interior of the sampling tube 'and thereafter The fluid reaction mixture was removed from the sampling tube to the outside of the reactor and analyzed. The sleeve used is usually a metal tube, which preferably has an outer diameter in the range of 5 to 15 mm, particularly 8 to 10 mm, and a wall thickness of preferably 1 mm. According to 97923.doc • 17- 200528191 = Invention 'The sleeve has a plurality of perforations (i.e., holes) toward the reaction space, and the temple holes are in principle unlimited with regard to its geometry. However, it is preferable to choose holes with α openings / shapes. Sheep 3 may also be slot-shaped with the slits arranged in the longitudinal direction of the sampling tube. These perforations preferably have the total surface area of the sleeve of the sleeve. 1 to 50/0, preferably no% of the total surface area. It is used to allow the fluid reaction mixture to flow into the sleeve and thus through the hole of the sleeve into a sampling tube placed inside the sleeve. The samples taken from the sampling tube outside the reactor can be analyzed by, for example, available factory analytical instruments. It is also possible to take samples and analyze the samples continuously or at specific intervals. The removal of the sample can be achieved by the autogenous pressure of the reaction system, which is generated by a control valve or an overflow device, or by a pump or a compressor or a radiator / ejector, in which case the sample can be introduced To a system with atmospheric pressure or a reduced or high pressure relative to the atmosphere. The preferred choice is to control the analysis system in which the sample is introduced with I · C-determined C force to increase the measurement accuracy. In a preferred embodiment, the perforated sleeve is centered in the gap. In this arrangement, the symmetry of the flow distribution in the gap is destroyed to a particularly small extent. It can be placed vertically from the top or bottom, and preferably from the same side of the reactor as the feed side of the fluid reaction mixture. In the embodiment in which a sleeve is provided and in each case the fluid reaction mixture is fed into the reactor from above, the sleeve is advantageously equipped with a plurality of perforations only in the area above the gap, especially up to its midpoint. . Because the sampling officer only extends up to the upper part of the sleeve, the point where the sample is taken through the hole for the purpose of determining the sample composition, so the sleeve placed below this point is 97923.doc -18- 200528191 The zone will bypass the external reaction mixture. This is prevented by providing multiple perforations in the sleeve only in the area above the gap. Coincidentally 'the sleeve can be placed and the fluid reaction mixture fed down into the reactor in each case' and the heat carrier can preferably be passed through a hot plate and the heat carrier can be partially or completely under reaction conditions boiled. The sampling tube may preferably be connected to the sleeve in a fixed manner in such a way that the hole of the sampling tube is directly placed on the perforation of the sleeve, and the silk sample tube and the hole of the sleeve therefore overlap. In another preferred embodiment, the sampling tube is rotatably placed in a perforated sleeve and has at least two holes on the surface of its jacket that are offset as follows: the fluid reaction mixture is always only Flow into the sampling tube through one of the holes. The hole of the sampling tube is preferably placed in its longitudinal direction as a slot, which allows more available maneuverable space when the sleeve is matched with the hole of the sampling tube. This embodiment allows samples to be taken by a single sampling tube from a plurality of points distributed at the height of the gap. In another preferred variant, each sampling tube has at least two, preferably two to four independent chambers, each of which has a hole, and the fluid reaction mixture passes through the perforations of the sleeve. Flowed into the well, and the fluid reaction mixture was removed from each chamber individually and analyzed. The cavities ^ are arranged next to each other or concentrically. The formation of two or more independent chambers in the sampling tube increases the number of measurement points at which samples of the fluid reaction mixture can be taken. A particularly preferred embodiment is that the sampling tube is provided with a plurality of chambers and is arranged around its longitudinal axis in a rotatable manner 97923.doc -19-200528191. In this way two or more, preferably four mutually offset slots of each chamber are allowed to accommodate the fluid reaction mixture to be placed, in which case the fluid reaction mixture is always only in each case only Flowed into each chamber through a hole. This example further increases the number of measurement points of the components used in the reaction mixture. In another preferred embodiment, two or more sampling tubes are provided, and each of the sampling tubes is fixedly connected to the sleeve in the following manner: the hole of each sampling tube is directly placed in the sleeve Perforations, and individual sampling tubes open at different heights in the gap. In addition, the sleeve itself can be configured as a sampling tube by: providing perforations only at points where there is a direct connection to a sampling tube in each case, and additionally in a different A single additional perforation is provided at the point of the opening of the sampling tube through which the fluid reaction mixture flows. Therefore, the method and equipment according to the present invention make it possible in a simple manner to obtain accurate knowledge of actual reaction events and actual temperatures (preferably also those that are critical to hot spots) using available plant analysis instruments. In this way, operations that are substantially closer to the load limit of the catalyst are allowed; therefore, the catalyst can be better utilized, while at the same time preventing damage caused by the formation of undesirable hot spots. In addition, according to the knowledge of actual reaction events, the catalyst activity can be spatially configured within the gap to match the changing pattern of the actual reaction events. Protecting the catalyst in this way, especially in areas with more thermal stress, and therefore better adjusting its aging for longer or more advantageous use. In addition, the reactor can operate substantially more uniformly, which can have a positive effect on the overall selectivity of the reactions in which 97923.doc -20-200528191 occurs. In addition, the adaptation of catalyst activity to the actual reaction event allows the required amount of heat carrier to be reduced. Hereinafter, the present invention will be described in detail with reference to the drawings. [Performance Mode] Fig. 1 shows a cross-sectional view of a reaction line having a hot plate 1 and an intermediate gap 2 into which a fixed catalyst bed has been introduced. In the preferred embodiment shown, the sleeve 3 is centrally positioned in the gap 2 and seals, for example, a thermal element 4 having 4 measuring points. The sleeve 3 and the thermal element 4 protrude out of the reactor through a nozzle in the reactor jacket. The cross-section in Fig. 1A illustrates the cylindrical geometry of a sleeve 3 having a thermal element 4 disposed therein. The illustration in FIG. 2 shows a cross section of the reactor in the longitudinal direction in the area 乂 between two hot plates (not shown). In the gap 2, a sleeve 3 having a heat element 4 is placed at its transverse boundary 6. An insulating element 5 is provided between the sleeve 3 and the lateral boundary of the gap 2. The 検 cross section in FIG. 2 illustrates the heat plate (including its fixing to the lateral boundary 6), and the cylindrical design of ㈣3 with the heat element 4 and the shape of the insulating element 5 suitable for design. Fig. 3 shows a schematic diagram of a cross section of another embodiment in which the sleeve 3 having the heat element 4 is arranged horizontally in the gap 2. As shown in Figs. The sleeve has perforations 7 near the ends which protrude into the gap, by which a sample of the reaction mixture can be taken. The illustration in Figure 4 shows a longitudinal section of another embodiment with a sleeve 3 having a perforation 7 in the sleeve 3 for taking a sample into a sampling tube 8. The sleeve 3 with the sampling tube 8 extends beyond the nozzle 9 and protrudes out of the reactor. The inspection section in Fig. 4A illustrates an embodiment of the sleeve 3 having the hole 7 and the sampling tube 8 in the section. Fig. 5 shows a schematic cross-section of a reactor having parallel hot plates and an intermediate gap 2. By way of example, the sleeve 3 is shown and protrudes into the gap 2 between the two hot plates 1 in its longitudinal direction, and the sleeve is opened outside the reactor by a nozzle 9 in the reactor sleeve. Figure 6 shows the distribution of two preferred welding points on the surface of the hot plate: in each case, it illustrates the heat corresponding to 5 times the separation of the welds on the horizontal axis and 5 times the column separation on the vertical axis. The rectangular surface cross section of the plate. The upper description in FIG. 6 shows a preferred welding point distribution having a total of 33 welding points on the surface section shown on a hot plate with 5 times the welding point separation and 5 times the column separation, and The lower description shows another preferred arrangement, which has 25 welds on a surface section of the same size. [Brief description of the figure] FIG. 1 shows a cross section of a reactor having hot plates, which have a centrally arranged sleeve for accommodating a thermal element in a longitudinal section. FIG. 1A is a cross-sectional illustration. 2 shows a cross-section of another embodiment of a sleeve having a lateral placement in a longitudinal section, FIG. 2A is a cross-sectional illustration, and FIG. 3 shows another embodiment of a sleeve having a horizontal placement in a gap in a longitudinal section, 3A is a cross-sectional illustration and FIG. 36 is a detailed description. FIG. 4 shows a cross-section of another embodiment having a sleeve with a perforation and a sampling tube in a longitudinal section, and FIG. .doc -22- 200528191 Figure 5 shows a diagrammatic illustration of the placement of an inventive sleeve in a hot plate module 'and Figure 6 shows a diagram of a preferred welding point distribution on the surface of the hot plate. In the figures, the same reference numerals indicate the same or corresponding features. [Description of main component symbols] 1 Hot plate 2 Clearance 3 Sleeve 4 Thermal element 5 Insulating element 6 Transverse boundary 7 Perforation 8 Sampling tube 9 Nozzle 97923.doc -23-

Claims (1)

200528191 十、申請專利範圍: 1 · 一種用於監視、控制及/或調節在一異質微粒催化劑存在 下一反應器内之一流體反應混合物之反應之方法,該反 應器具有垂直且彼此平行排列、同時在每一情況下均留 有一間隙(2)之兩個或兩個以上熱板,該異質微粒催化 劑係安置於該等間隙(2)内,且該流體反應混合物通過該 等間隙(2),該方法包括選擇一或多個溫度作為一監視、 控制及/或調節參數,該或該等溫度係在—或多個間隙⑺ 内於分佈在每一間隙⑺之高度上的一或多個量測點處量 測。 2.如吻求項1之方法,其中將一或多個間隙(2)内之該流體反 應混合物之組合物選作另一監視、控制及/或調節參數, ^該組合物係於分佈在每_間隙⑺之高度上的一或多個 量測點處測定。 3· -種用於進行如請求項1之方法之設備,其特徵為一套筒 (3)’該套筒係安置於該間隙⑺内且在該反應器外部打 開’且在每一情況下均密封一具有一或多個量測點之溫 度量測插件(4)。 月长員3之β又備’其中該套筒係在縱向上設置於該 (2)内。 ,、 5.如請求項3或4之設備’其中該等熱板⑴係安置於: _ ㈣熱板模組⑽内’其各由彼此平行排 歹J同4在母一情況下均留有一間隙⑺之兩個或兩個 以上矩形熱板(1)形成, 97923.doc 200528191 -该等熱板模組(10)完全由一釋放壓力之主要為圓柱形 的外殼(U、12、13)所包圍,該外殼包括一圓筒夾套(11) 及盍(12、13),其在兩個末端處封閉該外殼,且其縱軸 經對準成平行於該等熱板(1)之平面, 將一或多個密封元件(14、;[ 5)以使該流體反應混合物除 了流過由該等蓋(12、13)所界限之反應器内部外僅流過 該等間隙(2)之方式設置,及 -具有一或多個袓互獨立之溫度量測插件(4)之每一熱板 杈組(10)較佳配備有兩個或三個、更佳為三個溫度量測 插件(4)。 6·如凊求項3或4之設備,其中該溫度量測插件(句為一多重 量測插件,較佳為一多重熱元件。 7·如請求項3或4之設備,其中該套筒較佳為一金屬管,該 套筒尤其具有一在4至15毫米範圍内、較佳在6至1〇毫米 範圍内、更佳在6至8毫米範圍内之外徑,且進一步較佳 具有〇·8至1.5毫米、較佳為丨毫米之壁厚度。 8·如請求項3或4之設備,其中該套筒(3)在該反應器内部内 具有一或多個斷開點。 9·如請求項3或4之設備,其中該溫度量測插件(4)之該等量 測點係經設置成在具有預期溫度極限及/或特別大的溫度 梯度之反應器區域内彼此間具有一相對較小之分離度, 而在其餘反應器區域内彼此間具有一相對較大之分離 度。 10·如請求項3或4之設備,其中密封該溫度量測插件(4)之該 97923.doc 200528191 套筒(3)在該反應器上方與下方以如下方式打開:可使較 佳配備有等距量測點之該溫度量測插件(句在該套筒 内連績地移位,以用於不間斷地量測溫度分佈。 11 12. 13. 14. 15. 16. 17. 18. 如請求項3或4之設備,其中該溫度量測插件(4)具有5至6〇 個量測點,較佳具有10至50個量測點,更佳具有15至4〇 個量測點,且仍更佳具有2〇至3〇個量測點。 如請求項Η之設備,其中該溫度量測插件(4)具有2〇個量 測點及約3.8毫米之外徑,且該套筒(3)具有6毫米或1/4英 对之外徑及4¾米或5/32英对之内徑。 如請求項丨丨之設備,其中該溫度量測插件(4)具有4〇人個量 測點及約2.5毫米之外徑,且該套筒(3)具有5毫米或3/16 英对之外徑及3¾米或1/8英忖之内徑。 如請求項4之設備,其中該套筒(3)係在縱向上正中設置於 該間隙(2)内。 如請求項4之設備,其中該套筒(3)係設置於該間隙(幻之 橫向邊界(6)處。 如請求項15之設備,其中在該間隙⑺之該橫向邊界⑹與 該套筒(3)之間設置一絕緣元件,該套筒⑺較佳係以一固 定方式安置於該間隙(2)内,且該套筒(3)更佳具有一正方 形或半圓形截面。 如請求項3之設備,其中該套筒(3)係水平地設置於該間隙 (2)内。 :種用於進行如請求項2之方法之設備,其中,除了如請 求項3至16任一項中所界定之該設備外,在每一情況下, 97923.doc 200528191 在一或多個間隙(2)内提供一套筒(3),且該套筒具有穿孔 (7)以及用於引入至該套筒(3)中之至少一取樣管(8),該取 樣管係以如下方式設置於該套筒内:該流體反應混合 物流過該套筒(3)内之該等穿孔而進入該取樣管(8) 中’且自該取樣管中將該流體反應混合物移除至該反 應器外部,並對其加以分析。 19·如請求項18之設備,其中該取樣管(8)係以如下方式以一 固定方式連接至該套筒(3):該取樣管(8)之一孔係直接安 置於該套筒(3)之一穿孔(7)上。 20.如請求項18之設備,其中該取樣管(8)係以一可旋轉方式 設置於該穿孔的套筒(3)内,且具有設置於其夾套表面上 之以如下方式偏移的兩個或兩個以上之孔:該流體反應 混合物總是僅藉由該等孔中之一孔流進該取樣管(8)中。 21 ·如睛求項20之設備’其中將該取樣管(8)之該等孔設計成 在其縱向上之狹槽。 22·如請求項18之設備,其中每一取樣管(8)具有兩個或兩個 以上、較佳為2至4個相互獨立之腔室,每一腔室均具有 一孔,該流體反應混合物藉由該套筒(3)内之該等穿孔(7) 而流進該孔中,且將該流體反應混合物單獨自每一腔室 移除並對其加以分析。 23 ·如請求項22之設備,其中該等腔室係相互相鄰地或同心 地設置。 24·如請求項21之設備,其中將具有複數個腔室之該取樣管(8) 設計成可環繞其縱軸旋轉。 97923.doc 200528191 25·如明求項18之設備,其中提供兩個或兩個以上之取樣管 (8),且將該等取樣管以如下方式以一固定方式各連接 至省套筒(3):每一取樣管之該孔係直接設置於該套筒 (3)之一穿孔(7)上,且該等個別取樣管(8)在該間隙(2)内各 於一不同高度處打開。 26. 如請求項18之設備,其中將該套筒(3)本身設計成一取樣 管(8)。 27. —種用於將如請求項3之設備併入於一反應器中之方 法’其中該設備係自該反應器之與該流體反應混合物之 饋入側相同的側設置。 28. 如請求項27之方法,其中設置該設備,且在每一情況下 將該流體反應混合物自上方饋入至該反應器内,且該套 筒(3)僅在該間隙(2)之上部區域内,尤其在直至該間隙(2) 之中點附近具有穿孔(7)。 29·如請求項27之方法,其中設置該(該等)設備,且在每一情 況下將該流體反應混合物自下方饋入至該反應器内,且 較佳使一熱載體通過該等熱板(1)並在反應條件下使該熱 載體部分或完全蒸發。 97923.doc200528191 X. Scope of patent application: 1 · A method for monitoring, controlling and / or regulating the reaction of a fluid reaction mixture in a reactor in which a heterogeneous particulate catalyst is present, the reactors are arranged vertically and parallel to each other, At the same time, two or more hot plates with a gap (2) are left in each case. The heterogeneous particulate catalyst is placed in the gaps (2), and the fluid reaction mixture passes through the gaps (2). The method includes selecting one or more temperatures as a monitoring, controlling and / or adjusting parameter, the temperature or temperatures being within one or more of the gaps ⑺ distributed at the height of each gap ⑺ Measure at the measurement point. 2. The method of claim 1, wherein the composition of the fluid reaction mixture in one or more gaps (2) is selected as another monitoring, control and / or adjustment parameter, and the composition is distributed in Measured at one or more measurement points at the height of each gap. 3. A device for carrying out the method as claimed in claim 1, characterized by a sleeve (3) 'the sleeve is placed in the gap 且 and opened outside the reactor' and in each case All are sealed with a temperature measuring plug (4) having one or more measuring points. Β of the month officer 3 is also prepared, wherein the sleeve is arranged in the (2) in the longitudinal direction. , 5. If the equipment in item 3 or 4 is requested, where the hot plates are placed in: _ ㈣ hot plate module ', each of which is arranged in parallel with each other, J and 4 have one in the case of the mother. The gap 形成 is formed by two or more rectangular hot plates (1), 97923.doc 200528191-the hot plate modules (10) are completely composed of a mainly cylindrical shell (U, 12, 13) that releases pressure Enclosed, the shell includes a cylindrical jacket (11) and a cymbal (12, 13), which closes the shell at both ends, and its longitudinal axis is aligned parallel to the plane of the hot plates (1) , One or more sealing elements (14 ,; [5) so that the fluid reaction mixture flows through only the gaps (2) except through the interior of the reactor bounded by the covers (12, 13) Mode setting, and-each hot plate branch group (10) having one or more independent temperature measuring plugs (4) is preferably equipped with two or three, more preferably three temperature measuring plugs (4). 6. If the equipment of item 3 or 4 is sought, the temperature measurement plug-in (sentence is a multiple weight measurement plug-in, preferably a multiple thermal element. 7. If the equipment of item 3 or 4 is requested, wherein the The sleeve is preferably a metal tube, and the sleeve particularly has an outer diameter in the range of 4 to 15 mm, preferably in the range of 6 to 10 mm, more preferably in the range of 6 to 8 mm, and furthermore Preferably having a wall thickness of 0.8 to 1.5 mm, preferably 丨 mm. 8. The device as claimed in item 3 or 4, wherein the sleeve (3) has one or more break points in the interior of the reactor 9. The device according to claim 3 or 4, wherein the measuring points of the temperature measuring plug-in (4) are set to each other in the area of the reactor with the expected temperature limit and / or a particularly large temperature gradient There is a relatively small degree of separation between each other, and a relatively large degree of separation between each other in the remaining reactor area. 10. The device of claim 3 or 4, wherein the temperature measuring insert (4) is sealed. The 97923.doc 200528191 sleeve (3) is opened above and below the reactor in the following manner: Equipped with this temperature measurement plug-in with equidistant measurement points (sentences are successively shifted within the sleeve for continuous measurement of temperature distribution. 11 12. 13. 14. 15. 16. 17. 18. The device as claimed in item 3 or 4, wherein the temperature measuring plug-in (4) has 5 to 60 measuring points, preferably 10 to 50 measuring points, more preferably 15 to 40 measuring points. Measuring points, and still more preferably with 20 to 30 measuring points. If the device of item Η is requested, the temperature measuring plug (4) has 20 measuring points and an outer diameter of about 3.8 mm, and The sleeve (3) has an outer diameter of 6 mm or 1/4 inch pairs and an inner diameter of 4¾ meters or 5/32 inch pairs. The device as requested, wherein the temperature measuring insert (4) has 4 〇 Each measuring point and an outer diameter of about 2.5 mm, and the sleeve (3) has an outer diameter of 5 mm or 3/16 inch pairs and an inner diameter of 3¾ meters or 1/8 inch. As requested in item 4 Equipment of which the sleeve (3) is longitudinally centered within the gap (2). The device of claim 4, wherein the sleeve (3) is located within the gap (magic horizontal border (6) ). If the equipment of item 15 is requested, An insulating element is provided between the transverse boundary ⑹ of the gap ⑹ and the sleeve (3), and the sleeve ⑺ is preferably placed in the gap (2) in a fixed manner, and the sleeve (3) More preferably, it has a square or semi-circular cross section. The device as claimed in item 3, wherein the sleeve (3) is arranged horizontally in the gap (2) .: A device for performing the method as claimed in item 2 , Wherein, in addition to the device as defined in any of claims 3 to 16, in each case 97923.doc 200528191 provides a sleeve (3) within one or more gaps (2), and The sleeve has a perforation (7) and at least one sampling tube (8) for introduction into the sleeve (3), the sampling tube being arranged in the sleeve as follows: the fluid reaction mixture flows through the The perforations in the sleeve (3) enter the sampling tube (8) 'and the fluid reaction mixture is removed from the sampling tube to the outside of the reactor and analyzed. 19. The device of claim 18, wherein the sampling tube (8) is connected to the sleeve (3) in a fixed manner as follows: a hole of the sampling tube (8) is directly placed in the sleeve ( 3) One of the holes (7). 20. The device of claim 18, wherein the sampling tube (8) is rotatably disposed in the perforated sleeve (3), and has a biasing mechanism disposed on the surface of its jacket as follows. Two or more holes: The fluid reaction mixture always flows into the sampling tube (8) through only one of the holes. 21-The device of the item 20 as described above, wherein the holes of the sampling tube (8) are designed as slots in the longitudinal direction thereof. 22. The device of claim 18, wherein each sampling tube (8) has two or more, preferably two to four independent chambers, each of which has a hole, and the fluid reacts The mixture flows into the holes through the perforations (7) in the sleeve (3), and the fluid reaction mixture is individually removed from each chamber and analyzed. 23. The device of claim 22, wherein the chambers are arranged adjacent to each other or concentrically. 24. The device of claim 21, wherein the sampling tube (8) having a plurality of chambers is designed to be rotatable about its longitudinal axis. 97923.doc 200528191 25 · If the equipment of item 18 is provided, two or more sampling tubes (8) are provided, and the sampling tubes are each connected to the provincial sleeve (3) in a fixed manner as follows: ): The hole of each sampling tube is directly set on a perforation (7) of the sleeve (3), and the individual sampling tubes (8) are opened at different heights in the gap (2). . 26. The device of claim 18, wherein the sleeve (3) is itself designed as a sampling tube (8). 27. A method for incorporating equipment as claimed in claim 3 in a reactor, wherein the equipment is provided from the same side of the reactor as the feed side of the fluid reaction mixture. 28. The method of claim 27, wherein the device is provided, and in each case the fluid reaction mixture is fed into the reactor from above, and the sleeve (3) is only in the gap (2). There are perforations (7) in the upper region, especially up to the midpoint of the gap (2). 29. The method of claim 27, wherein the device (s) are provided, and in each case the fluid reaction mixture is fed into the reactor from below, and preferably a heat carrier is passed through the heat Plate (1) and partially or completely evaporate the heat carrier under reaction conditions. 97923.doc
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