TWI376267B - 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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TWI376267B
TWI376267B TW93138975A TW93138975A TWI376267B TW I376267 B TWI376267 B TW I376267B TW 93138975 A TW93138975 A TW 93138975A TW 93138975 A TW93138975 A TW 93138975A TW I376267 B TWI376267 B TW I376267B
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reactor
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gap
reaction mixture
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TW200528191A (en
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Gerhard Olbert
Claus Hechler
Dietmar Loewen
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Basf Ag
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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
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    • 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
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    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
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    • B01J2208/00628Controlling the composition of the reactive mixture
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • 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
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    • 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
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    • 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
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    • 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)

Description

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 反應器内之流體反應混合物之反應之方法,太 i不"W明亦係 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 化劑管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0 作為一替代,亦可經由通過板型熱轉移器之熱載體來移 除反應之熱量。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 内部具有入口及出口管線,且與表面區域相比具有較薄之 厚度。該等熱轉移器板通常係由金屬薄片製造,經常係由 鋼薄片製造。然而’視應用情況而定,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。用於熱載體之入口及出口裝置通常排列 97923.doc 1376267 於熱交換器板之相對端處。所用之熱載體經常為水或 Diphyl®(a重量計70至75%之二苯醚與以重量計以至3〇%之 聯苯的混合物)’該等熱載體有時亦會在煮沸作業(b〇iUng 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 418t。優先選擇含有硫酸鹽、磷酸鹽、硼酸 鹽或梦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 啶鑌或鱗陽離子之離子性液體亦是有利的。 術語熱板待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(roll 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^。IX. INSTRUCTIONS OF THE INVENTION: TECHNICAL FIELD OF THE INVENTION The present invention relates to a method for monitoring, controlling and/or regulating the reaction of a fluid reaction mixture in a reactor having a hot plate, too i not "W Ming It relates to a device for carrying out the method. [Prior Art] Many reactions (especially partial oxidation reactions) of 'fluids (meaning gas, liquid or gas/liquid reaction mixtures) are known in chemical processing techniques. 'These reaction systems are present in heterogeneous particulate catalysts. In the case of the case. These reactions are usually exothermic and often strongly exothermic. It has heretofore been carried out on an industrial scale mainly in a tube bundle reactor having a catalyst tube, into which a heterogeneous particulate catalyst is introduced, and the fluid reaction mixture passes through the catalyst tubes and the heat released by the reaction is via The heat carrier circulating in the intermediate space between the catalyst tubes is indirectly removed. The heat carrier used is often an alternative to the salt melt 0, and the heat of the reaction can also be removed via a heat carrier through a plate type heat transfer device. The terms heat exchanger plate, heat transfer plate and hot plate are used synonymously for a plate type heat transfer device. The heat transfer plate is primarily defined as having an inner sheet-like structure with inlet and outlet lines and a thinner thickness than the surface area. These heat transfer plates are typically made of sheet metal, often made of steel sheets. However, depending on the application, depending on the nature of the reaction medium and the heat carrier, specific, particularly corrosion-resistant, or coated materials may be used. The inlet and outlet means for the heat carrier are typically arranged at 97923.doc 1376267 at the opposite end of the heat exchanger plates. The heat carrier used is often water or Diphyl® (a mixture of 70 to 75% diphenyl ether by weight and up to 3% by weight of biphenyl). These heat carriers are sometimes also used in boiling operations (b Evaporation in 〇iUng 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 418t. An ionic liquid containing a sulfate, a phosphate, a borate or a dream acid anion is preferred. Ionic liquids containing a monovalent metal cation (especially an alkali metal cation) and another cation (particularly an imidazolium cation) are also particularly suitable. It is also advantageous to contain an ionic liquid of imidazolium, pyridinium or scaly cation as a cation. The term hot plate is used in heat transfer plates where a single (usually two) foil is joined together by spot welding and/or roll weld, and the water is often used to plasticize the sheet. The ground is shaped to form a recess ^.

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 混合物於一反應器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 1376267 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,根據該申嗜 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 设。包裝板組件無需在圓周側上適應,且因此可以至圓柱 形反應器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 01/85 331中。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,其中該等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: _ 一或多個立方形熱板模組,其各由彼此平行排列、同時 在母清’兄下均留有間隙之兩個或兩個以上矩形熱板形 成°亥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 1376267 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。 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之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f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’該或該等溫度係在一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。 根據本發明,所選擇之監視、控制及/或調節參數為一或 多値溫度,該或該等溫度係在一或多個間隙内於分佈在^ 97923.doc -9. 1376267 一間隙之高度上的—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内之 之組份作為另一的葙、批制芬,士 久應此5物 每一門隙^ 制及或調節參數,其係於分佈在 母間隙之向度上的一或多個量測點處得以判定。In this context, the terms heat exchanger plate, heat transfer plate and hot plate are used in the sense defined above. A reactor system for the partial oxidation of a hot plate is known, for example, from DE-A 199 52 964. This application describes the arrangement of catalysts for partial oxidation in a reactor on a bed around a heat transfer plate. The reaction mixture is fed at a reactor end to the interior of the reactor between the heat transfer plates and removed at the opposite end, and it thus flows through the intermediate space between the heat transfer plates. DE-C 197 54 185 describes another reactor 'which indirectly removes heat via a cooling medium flowing through a heat transfer plate, which is designed as a hot plate composed of at least two steel plates 97792.doc 1376267 The steel sheets are joined together at predetermined points to form a flow passage. An advantageous development is described in DE-A 198 48 208, according to which a heat transfer plate configured as a hot 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 peripherals. The packaging panel assembly need not be adapted on the circumferential side and can therefore be used at a predetermined spacing from the inner wall of the cylindrical reactor vessel. A free surface between the plate heat transfer device or its outer casing and the inner wall of the container is covered by a guide plate in the upper and lower regions of the outer casing to prevent the reaction medium from bypassing the chamber filled with the catalyst. Another reactor having means for removing heat from the reaction in the form of a plate heat transfer is described in WO-A 01/85 331. The reactor, which is primarily cylindrical in shape, contains a continuous catalyst bed in which a plate heat transfer device is embedded. DE-A 103 33 866 discloses the problems occurring as a result of the deformation and the prevention of mechanical stability as a result of reshaping under high thermal stress, wherein the deformation exists between the reaction mixture and the external environment. As a result of the high stress on one side of the hot plate in the case of an excessively high pressure difference, the reaction mixture is subjected to a high pressure or by providing a reactor for partially oxidizing the fluid reaction mixture in the presence of a heterogeneous particulate catalyst These mechanical stability problems may occur when decompressing. The reactor has: _ one or more cubic hot plate modules, each arranged in parallel with each other, while leaving a gap under the mother's brother Two or more rectangular hot plates may be formed to fill the gap with a heterogeneous particulate catalyst, and the fluid reaction mixture flows through the gap, and the heat of the reaction flows through the hot plates and is 97923.doc 1376267, thus at least partially Evaporating the heat carrier for absorption; the reactor has: - a predominantly cylindrical outer casing that releases pressure at the hot plate module and completely surrounds the a module, and comprising a cylindrical jacket and a hood, the outer casing is closed at both ends, and the longitudinal axis thereof is aligned parallel to the plane of the hot plate; and the reactor also has: - one or more A sealing element arranged in such a manner that the fluid reaction mixture flows only through the gaps beyond the internal 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 the reaction of a fluid reaction mixture carried out in a reactor having a hot plate disposed therein, heterogeneous particles The catalyst is disposed in the gap between the hot plates and flows through the reaction medium, and the heat carrier flows through the hot plates. Thus, we have discovered a method for monitoring, controlling and/or regulating the reaction of a fluid reaction mixture in a reactor in the presence of a heterogeneous particulate catalyst, the reactors being vertically and parallel to each other, in each case Two or more hot plates with a gap left, the hetero-f particulate catalyst disposed within the gap, and the fluid reaction mixture passing through the gaps, the method comprising selecting one or more temperatures as a monitoring, control, and/or The adjustment parameter 'the or the temperature is measured at one or more measurement points distributed over the height of each gap in one or more gaps. According to the invention, the selected monitoring, control and/or adjustment parameters are one or more temperatures, which are distributed in one or more gaps at a height of ^ 97923.doc -9. 1376267. The above - or multiple measurement points are measured. Preferentially, the component of one or more gaps is additionally selected as another 葙, batch fen, and the time interval of each of the five objects is controlled and adjusted, which is distributed in the direction of the mother gap. One or more measurement points at the degree are determined.

知=Γ運行條件之判定,催化劑床中之溫度場的 =實:重要的。此涉及溫度之局部分佈亦及(例如)溫度 取大值(熱點)之量值與位置。沿反應介質之流動路徑的溫度 分佈對於反應系統之控制及調節而言亦可能很重要。X 除穩態運行外,亦必須控制啟動或停止或(例如)甚至超 過延長時期仍會隨時間而變化之運行的邊界條件,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纟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(throughput)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中 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· 1376267 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’尤其為氡化或部分氧化反應。 >•、有熱板之反應益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、1.4571 或 1.4406、1.4539 或 1.4547 與1.4301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1與4毫米、15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 焊接接頭或此等兩者之组合,使得其中稍後安置有熱載體 之空間在所有侧上被密封。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)且其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35 97923.doc -11- 1376267 至7〇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50毫米以及46至48 毫米之分離度。通常,由於製造之結果,點分離度會變化 多達±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排列。板之縱向方向 上之點焊之列可以5至50毫米或8至25毫米之分離度等距排 列’雖然亦可使用10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 中熱板有一定的均勻膨脹。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3 000個焊接點/平方米板表面積,典型值為丨4〇〇 至2600個焊接點/平方米板表面積。有利地,在5倍之焊接 點勿離度乘5倍之列分離度之矩形表面截面上存在2〇至35 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500與1500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3000與4〇〇〇毫米 之間。 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1〇至1〇〇毫米之寬度。一可能之實施例亦具 97923.doc 12 1376267 有12至50毫米或14至25毫米之寬度,雖然亦可選心6至2() 毫米之寬度。亦已測試了 17毫米之間隙分離度。 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 圓形卷狀接缝或焊接點而自熱載體之流動 之—)能夠將截面中間之孔引入至用於桿= 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 應允許或所要之反應需要、或可達成設備或冷卻技術:點 時,該等間隙亦可具有不同的寬度。 ”.、板模組之以催化劑微粒填充之間隙可相對於彼此密 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一起以形成模組時調整所要之 間隙刀離度’將該等板固定於其位置中並以分離度固定。 直接相鄰之熱板之焊接點可彼此相對或彼此偏移。 月亦提供一用於進行上文所述之方法之設備,其以. ,筒為特徵,該套筒安置於兩個熱板間之間隙内,較佳 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: 昉5 —個立方形熱板模組十,其各由彼此平行排列、同 卜匱况下均留有間隙之兩個或兩個以上矩形埶板 形成, … 97923.doc 1376267 _熱板模組完全由釋放壓力之主要為_形的外 圍,該外殼包括圓筒夾套及蓋,其於兩個末端處封閉該 外殼,且其縱軸對準成平行於熱板之平面, --或多個密封元件以流體反應混合物除了流過由該等蓋 所界限之反應器内部外僅流過該等間隙之方式排列及 -具有-或多個相互獨立之溫度量測插件之每一熱板模組 較佳均配備有兩個或二個、p /土色_ 丨U 4 一彳回更仏為二個溫度量測插件。 根據在每-情況下均配備有至少一獨立之溫度量測插件 2每-熱板模組,可個別地評估並監視每_熱板模組。為 每-熱板模組提供-個以上溫度量測插件係有利的,使得 在個別溫度量測插件失效之情況下,仍能確保安全運行。 當在每m每熱板模組上使m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10毫米、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14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 上係與可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*** 於催化J床中時’有必要在管束反應器之情況下使用具有 =之内徑之特別製造的管,以使反應分佈能夠等同:此 寻目中之剩餘正常反應管中之反應分佈,且因此等同於代 97923.doc -U· 表性溫度量測》 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7L件之套筒中心地在其縱轴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-A 101 10 847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 板間之間隙内之該等特定排列來量測催化劑床内之溫度分 佈。 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。 溫度量測插件或套筒與兩個熱板之距離在每一情況下較 佳可相等,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。 套筒可在反應器外部在其上與其下打開。在一較佳實施 例中’套筒可在反應器上與在其下打開。在該情況下,可 使/ja度量測插件在套筒内連續地移位,使得不僅可判定離 散溫度量測’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 具有等距量測分離度之多重量測元件,因為用於不間斷地 97923.doc -15- 1376267 量測溫度分体之必要移位路徑因而僅為一量測點分離度。 套筒可被無鏠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入之情況下在熱 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夹環式連接,使得顯著較容易地製成 组件。Knowing the determination of the operating conditions, the temperature field in the catalyst bed = actual: important. This involves the local distribution of temperature and, for example, the magnitude and location of the temperature taking a large value (hot spot). The temperature distribution along the flow path of the reaction medium may also be important for the control and regulation of the reaction system. In addition to steady-state operation, X must also control the boundary conditions of the operation that initiates or stops or, for example, even changes over time, such as changes in catalyst activity (deactivation). Based on the measured temperature, it is possible, for example, to ensure safe operation and to control and maintain optimal operating conditions that are better in the first case. It can be concluded, for example, about the optimal operating mode of the reactant component and reactant flow rate, as well as the cooling temperature and the throughput of the cooling medium. Furthermore, the additional concentration measurement in the catalyst bed allows monitoring of the distribution of the material in the reaction. And, for example, also allows for the determination of reaction kinetics under operating conditions. For example, the deactivation behavior of the catalyst can also be characterized according to the concentration distribution during the circulation, in particular together with the temperature distribution. It can also be used for low by-product formation by adapting to reactant loading and processing flow rates. Advantageous reaction control, or improvements in catalyst and reactor design. The inventors have recognized that 'the temperature distribution at the height of the particulate catalyst that has been introduced into the gap between the two hot plates can be determined without the measurement operation itself interfering with the method (ie, along the flow) Temperature distribution of the path), 97923.doc • 10· 1376267 Also the concentration distribution at the height of the catalyst (ie, the concentration distribution along the flow path). There is in principle no limitation on the chemical reaction that can be monitored, controlled and/or regulated by the method according to the invention in the presence of a heterogeneous particulate catalyst in the presence of a heterogeneous particulate catalyst. Preferably, the reaction is a reaction of the gaseous reaction mixture, especially a deuteration or partial oxidation reaction. >•, the reaction benefits of hot plates have been described above. The hot plate is preferably made of a non-corrosive material, in particular made of, for example, stainless steel having material numbers 1.4541 or 1.4404, 1.4571 or 1.4406, 1.4539 or 1.4547 and 1.4301, or other alloy steel. The thickness of the material of the foil used for this purpose may be between 1 and 4 mm, between 15 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 create a hot plate, in which case there may be a roll seam or a transverse weld joint or a combination of the two, such that The space in which the heat carrier is placed is sealed on all sides. The edges of the hot plate are advantageously removed at or even within the transverse seam of the longitudinal edges such that the cooling is poor (if complete) and the edge regions in which the catalyst has typically been placed have a very low geometric expansion. The metal foil is joined by spot welding distributed on a rectangular surface. There may also be at least partial partial connections that are connected by straight or curved and circular rolled seams. It is also possible to divide the volume through which the heat carrier flows by a plurality of separate seams into a plurality of separate regions. One of the possibilities of arranging the solder joints on the hot plate is arranged in a column having an equidistant point resolution of 3 〇 to 8 〇 mm or 35 97923.doc -11 - 1376267 to 7 〇 mm, although it may be 4 〇 to A resolution of 6 mm, and another embodiment has a resolution of 45 to 50 mm and 46 to 48 mm. Generally, as a result of the manufacturing, the dot resolution varies by as much as ±1 mm' and, in the longitudinal direction of the panel, the solder joints adjacent to the columns are arranged in such a manner as to offset half of the solder joint resolution. The spot welds in the longitudinal direction of the sheet can be arranged equidistantly from 5 to 50 mm or from 8 to 25 mm apart, although separations of 10 to 20 mm and 12 to 14 mm can also be used. In addition, there may be a pair of solder joint resolution and column resolution mentioned in the application. The column resolution may be a certain geometric relationship with the point separation degree, which is usually V4 or slightly lower than the point resolution. In order to make the hot plate have a certain uniform expansion during the manufacturing process. For a given weld point and column separation 'specify a certain number of weld points per board surface area; possible values are 200 to 3,000 welds per square meter of surface area, typically 丨4〇〇 to 2600 Solder joint / square meter surface area. Advantageously, there are 2 to 35 weld points on a rectangular surface section of 5 times the degree of separation by 5 times the degree of separation. The width of the hot plate is generally limited by manufacturing techniques and may be between 100 and 2500 mm or between 500 and 1500 mm. The length of the hot plate depends on the reaction, in particular on the temperature distribution of the reaction' and the length can be between 500 and 7000 mm or between 3000 and 4 mm. In each case, two or more hot plates are arranged in parallel and separated from each other to form a hot plate module. In this way, a rod-like gap formed between the plates is produced. The heat plates have, for example, a width of between 8 and 150 mm or a width of 1 to 1 mm at the narrowest point of the plate separation. A possible embodiment also has 97923.doc 12 1376267 having a width of 12 to 50 mm or 14 to 25 mm, although a width of 6 to 2 () mm is also selectable. A gap separation of 17 mm has also been tested. A plurality of spacers may be additionally disposed between individual hot plates of the hot plate module, such as in the case of large surface area plates, to prevent deformation of the plate separation or position. To accommodate the spacers, the hole in the middle of the section can be introduced into the plate for the rod = sheet, for example, by the flow of the heat carrier by a large diameter circular seam or weld. The spacers may be fixed by screws or solder. The gaps between individual panels may have the same degree of separation, but (if desired) the gaps may also have different widths when the reaction allows or requires the desired reaction, or equipment or cooling techniques can be achieved: point. The gaps of the plate modules filled with catalyst particles may be sealed relative to each other, for example by welding, or joined together on the processing side. In order to adjust the individual hot plates together to form a module The gap knife degree 'fixes the plates in their position and is fixed by the degree of separation. The solder joints of the immediately adjacent hot plates may be opposite to each other or offset from each other. The month also provides a The apparatus of the method is characterized in that the sleeve is disposed in a gap between two hot plates, preferably in a direction, and opens and seals the temperature measuring insert outside the reactor, for example, having _ or more One of the measuring points or a plurality of thermal elements. The hot plate is preferably disposed in: 昉5—a cubic hot plate module ten, each of which is arranged in parallel with each other, and has two gaps in the same state. Or more than two rectangular slabs are formed, ... 97923.doc 1376267 _The hot plate module is completely surrounded by the _-shaped outer periphery of the release pressure, the outer casing comprises a cylindrical jacket and a cover which closes the outer casing at both ends And its longitudinal axis is aligned parallel to the heat a flat surface, or a plurality of sealing elements arranged in such a manner that the fluid reaction mixture flows through the gaps only outside the interior of the reactor bounded by the covers and has - or - a plurality of independent temperature measurements Each hot plate module of the plug-in is preferably equipped with two or two, p / earth color _ 丨 U 4 one turn back to two temperature measuring plug-ins. According to each case - at least A separate temperature measurement plug-in 2 per-hot plate module can individually evaluate and monitor each _ hot plate module. It is advantageous to provide more than one temperature measurement plug-in for each-hot plate module, so that When the temperature measurement plug-in fails, it can still ensure safe operation. When the m-measurement plug-in is made every m hot plate module, it may be in the case of testing, maintenance or failure of the temperature measurement plug-in, especially Maintaining safe operation when the temperature signal function is used to protect the circuit. The sleeve is a preferred metal tube, which in particular has a range of 4 to 15 mm, in particular 6 to 10 mm, often 6 to 8 mm. a diameter, and further preferably having a height of from 0.8 to 1.5 mm, preferably Wall thickness of 14 m. Although the sleeve and the hot plate do not have to be made of the same material, the material that can be used for the sleeve is in principle the same material as that which can be used for the hot plate. Non-ferrous materials can also be used as sleeves. According to the prior art, when a temperature measuring sleeve or a temperature measuring insert is inserted into a catalytic J bed, it is necessary to use a specially manufactured tube having an inner diameter of = in the case of a tube bundle reactor to make the reaction The distribution can be equivalent: the distribution of the reaction in the remaining normal reaction tubes in this search, and therefore equivalent to the generation 97923.doc -U· phenotypic temperature measurement, although compared to the reaction tube without the sleeve, for accommodation The usual arrangement of the sleeves of the 7L piece in the reaction tube centered on its longitudinal axis results in a high degree of distortion of the flow and temperature distribution, and therefore requires a reaction tube, a catalyst charge and, for example, a different wall thickness in cross section. A particular configuration of the sleeve or a particular arrangement of the sleeve within the catalyst tube, as described in DE-A 101 10 847, but it has been found that, surprisingly, a reactor with a hot plate does not necessarily require a gap between the hot plates. Such a specific arrangement to measure the temperature distribution within the catalyst bed. It is only necessary to place the temperature measuring insert itself or the sleeve sealing the temperature measuring insert in the gap, preferably in the longitudinal direction between the two hot plates. The distance between the temperature measuring insert or sleeve and the two hot plates is preferably equal in each case, meaning that 'in one embodiment, the temperature measuring insert is centrally disposed within the gap>> in order to introduce the sleeve into In the gap between the hot plates, it is particularly advantageous when the hot plates each have the same pattern of solder joints and the solder joints of adjacent hot plates are opposite each other. The sleeve can be opened on and off the outside of the reactor. In a preferred embodiment, the sleeve can be opened on and under the reactor. In this case, the /ja metrology insert can be continuously displaced within the sleeve so that not only the discrete temperature measurement can be determined but also a continuous description of the temperature distribution can be determined. For this purpose, an individual measuring element can be used, but it is also advantageous to use a multi-weight measuring element which is particularly advantageous for equidistant measurement of the degree of separation, since it is used for uninterrupted measuring of the temperature of the 97923.doc -15-1376267 The necessary displacement path of the body is thus only a measure of the degree of separation. The sleeve can be guided flawlessly through the outer reactor jacket or in the region above the hot plate module where the catalyst is loaded or in the region below the hot plate module with the connecting element. In a particularly advantageous variant, the sleeve has a break point inside the reactor, which is specifically designed as a cut-ring or clip-on connection, making the assembly significantly easier.

溫度量測插件通常具有分佈在其長度上並因&分佈在間 隙之高度上的複數個量測點。雖然亦可使用諸如鉑電阻溫 度計(例如PT· i 00或PT_ i _)、f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中之全部熱元件,較佳為根據DINEN6〇584tK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,較佳且有ι〇 至50個量測點,更佳具有15賤個量測點,且仍更佳具有 20至30個量測點。 在一較佳實施例中,溫度量測插件具有2G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—具有^ 97923.doc -16- ^/6267 米或1/4英忖之外徑及4毫米或咖英时之内徑的套筒内。 在另一較佳實施例中’溫度量測插件具有40個量測點及 ,·.勺2.5毫来之外徑’使得該溫度量測插件可安置於一具有5 毫米或3—m英奴外徑及3毫米或1/8英叶之内徑的套筒内。 貫%例t &封熱元件之套筒可安置於兩個敎板間 之間隙之橫向邊界處。為防止量測失真,在該情況下優先 選擇係在間隙之橫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:#筒以固定方式安置於間隙内並保 持在被處,不必將該套筒連同催化劑裝料—起安置並移 除。在該情兄下,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’亦可將冑封溫度量測插件之套筒水平地安置於兩 個熱板間之間隙内。以此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卜除上文所描述之具 有溫度量測插件之套筒外,在每一情況下,在一或多個間 '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^之至少一取樣管’該取樣管以如下方式安置於彼 ^ .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10毫米範圍内之外徑及較佳為i毫米之壁厚度。根據 97923.doc 17 1376267 本發明,套筒昇有朝著反應空間之多個穿孔(意即,孔),該 等孔原則上關於其幾何形狀無限制。然而優先選擇具有 圓形形狀之扎。詳言之’亦可能為狭槽排列在取樣管之縱 向方向上之狹槽形形狀。該等穿孔較佳具有套筒之總的夹 套表面積之1至50%、較佳為n〇%的總表面積。其用於允 許=體反應昆合物流進套筒内,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I以特㈣間間隔隸取樣品並分析樣品。 樣:之取出可由反應系統之自生壓力來實現,該自生壓力 裝置、或藉由泵或壓 射器來產生’在該情況下,可將樣品引入至-具有:氣厂: 或相對於.亥大氣之減壓或高壓的系統中。優先選擇係以 怪定壓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。 在女置有套筒且在每-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、尤其冋違其中點附近有利地配備有多個穿孔。由於取 樣e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 1376267 筒的空白區域將另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。 類似地’可安置套筒並在每一情況下將流體反應混合物 自下部饋入至反應器内’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,且取樣管與套筒之孔 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 的套琦内,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* 該實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—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。該等腔室可 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- 1376267 方式環繞其縱軸設置。以此方式允許每一腔室之兩個或兩 上、較佳為四個相互偏移狹槽容納待安置之流體反應 w σ物,在該情況下,流體反應混合物在每一情況下總是 僅糟由-孔而流進每_腔室中。該實施例進一步增加了用 於流體反應昆合物《組份的量咖之數目。 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S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;^不同的南度處打開。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 不同於取鮮n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载極限的操作;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間隙 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。 此可對於其中發 另外’反應器可大體上更均勻地運作 97923.doc •20· 1376267 生之反應的總選擇性產生正面的影響。另外,催化劑活十生 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。 【實施方式】 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之反應器之截面的圖解。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通過反應器套中之喷嘴而突出於 反應器外。 圖1Α中之橫截面說明了具有安置於其中之熱元件4之套 清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2之 區域内於縱向方向上之反應器的戴面。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中之橫截面說明了熱板丨(包含其對橫向邊界6之固 定)、亦及具有熱元件4之套筒3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’ s亥套筒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超過喷嘴9而突出於該反 97923.doc -21 - 1376267 應器外。 圖4 A中之橫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1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 喷嘴9而在反應器外部打開。 圖6顯示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^ 尺寸之表面戴面上具有25個焊接點。 【圖式簡單說明】 圖1顯示-具有熱板之反應器的截面,該等熱板在縱向截 ,内具有-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方 例的載面,圖2A中為橫截面說明, 圖3一顯示在縱向截面内具有水平安置於間隙内之套筒白 另貫施例,圖3A中為橫截面說明且圖3B中為詳細說明 圖4顯示在縱向戴面内具有一具有穿孔及取樣管之套f 之另-實施例的截面,圖4A中為橫戴面說明, ' 97923.doc -22- 1376267 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 噴嘴 97923.doc -23·Temperature measurement inserts typically have a plurality of measurement points distributed over their length and distributed at the height of the gap by & Although it is also possible to use all other (especially physical) temperature measurement principles such as platinum resistance thermometers (eg PT·i 00 or PT_i _), f-resistance thermometers or semiconductor sensors, useful temperature measurement inserts are preferred. It is a multi-weight measuring plug (called multiple thermal elements). Depending on the temperature used, useful thermal elements are all of the thermal elements described in DIN 43710 & DIN EN 60584, preferably in accordance with DIN EN 6 〇 584 tK type thermal elements. The distributed measuring points can be arranged equidistantly, but in a region of the reactor having a desired temperature limit and/or a particularly large temperature gradient, there is a relatively small degree of separation from one another and in the remaining reactor regions to each other It is particularly advantageous to have a relatively large degree of separation to arrange the equal measuring points. The temperature measuring insert advantageously has 5 to 6 量 measuring points, preferably ι〇 to 50 measuring points, more preferably 15 量 measuring points, and still more preferably 20 to 30 measuring points. point. In a preferred embodiment, the temperature measuring insert has 2G measuring points and an outer diameter of about 3.8 mm so that the temperature measuring insert can be placed at - 97923.doc -16-^/6267 meters or 1 /4 inches of outer diameter and 4 mm or the inner diameter of the sleeve. In another preferred embodiment, the 'temperature measuring insert has 40 measuring points and the outer diameter of 2.5 millimeters' so that the temperature measuring insert can be placed in a 5 mm or 3-m innocent The outer diameter and the inner diameter of the sleeve of 3 mm or 1/8 inch. The sleeve of the % of the t & heat sealing element can be placed at the lateral boundary of the gap between the two jaws. In order to prevent measurement distortion, in this case it is preferred to provide an insulating element between the lateral boundary of the gap and the sleeve so that a representative temperature signal can be obtained at the edge of the bed. In this case, it is particularly advantageous that the #cylinder is placed in the gap in a fixed manner and held in place, and it is not necessary to place and remove the sleeve together with the catalyst charge. In this case, the sleeve can also be designed to have a non-cylindrical geometry, for example having a square or semi-circular cross section. Alternatively, the sleeve of the sealing temperature measuring insert can be placed horizontally in the gap between the two hot plates. In this way it is allowed to determine the temperature distribution over the section of the gap. In another preferred embodiment of the inventive device, in addition to the sleeve having the temperature measuring insert described above, in each case a sleeve is provided in one or more compartments and the sleeve is provided The cartridge has a plurality of perforations and at least one sampling tube for introduction into the sleeve. The sampling tube is disposed in the manner that the fluid reaction mixture flows through the perforations in the sleeve into the interior of the sampling tube, and Thereafter the fluid reaction mixture was removed from the sample tube to the outside of the reactor and analyzed. The sleeve used is typically a metal tube which preferably has an outer diameter in the range of 5 to 15 mm, particularly 8 to 10 mm, and preferably a wall thickness of 1 mm. According to the invention, in accordance with the invention, the sleeve is provided with a plurality of perforations (i.e., holes) facing the reaction space, which are in principle unrestricted with respect to their geometry. However, it is preferred to have a round shape. In detail, it may also be a slot-like shape in which the slots are arranged in the longitudinal direction of the sampling tube. Preferably, the perforations have a total surface area of from 1 to 50%, preferably n%, of the total jacket surface area of the sleeve. It is used to allow the body reaction to flow into the sleeve and thus into the sampling tube disposed inside the sleeve via the bore of the sleeve. Samples taken from the sampling tube outside the reactor can be analyzed by, for example, available factory analytical instruments. It is also possible to continuously take samples and analyze samples at intervals of special (iv). Sample: the removal can be achieved by the autogenous pressure of the reaction system, the autogenous pressure device, or by pump or ejector to produce 'in this case, the sample can be introduced to - with: gas plant: or relative to. In a system of atmospheric decompression or high pressure. Preference is given to controlling the analysis system in which the sample is introduced with a strange pressure to increase the measurement accuracy. In a preferred embodiment, the perforated sleeve is centrally disposed within 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 is preferably placed from the same side of the reactor as the feed side of the fluid reaction mixture. In embodiments in which the sleeve is placed on the female and in each case the fluid reaction mixture is fed from the upper part into the reactor, the sleeve is advantageously provided only in the region above the gap, in particular in the vicinity of the point. Perforation. Since the sample e extends only in the upper region of the sleeve up to the point at which the sample is taken by the hole for the purpose of determining the sample component, the blank area of the sleeve set under the 97923.doc 1376267 will be additionally composed. Bypass of the reaction mixture. This is prevented by providing a plurality of perforations in the sleeve only in the upper region of the gap. Similarly, 'the sleeve can be placed and in each case the fluid reaction mixture fed from the lower part into the reactor' and the heat carrier can preferably be passed through a hot plate and the heat carrier partially or completely boiled under the reaction conditions . The sampling tube can preferably be attached to the sleeve in a fixed manner in such a manner that the hole of the sampling tube is placed directly on the perforation of the sleeve, and the sampling tube and the hole of the sleeve thus overlap. In another preferred embodiment, the 'sampling tube is rotatably disposed within the perforated sleeve and has at least two apertures disposed on the surface of the jacket that are offset in such a manner that the fluid reaction mixture is always only Flow through one of the holes into the sampling tube. The aperture of the sampling tube is preferably placed as a slot in its longitudinal direction, which allows for more available maneuvering space when the sleeve is mated with the aperture of the sampling tube. * This embodiment allows self-distribution by a single sampling tube Samples were taken at a plurality of points at the height of the gap. In another preferred variation, each sampling tube has at least two, preferably two to four, mutually independent chambers, each chamber having a bore, the fluid reaction mixture being perforated by the sleeve Flow into the well and the fluid reaction mixture was removed from each chamber separately and analyzed. The chambers may be arranged adjacent to each other or concentrically. The formation of two or more separate chambers within the sampling tube increases the number of measurement points at which a sample 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 further disposed about its longitudinal axis in a rotatable manner 97923.doc -19- 1376267. In this way, two or two, preferably four, mutually offset slots of each chamber are accommodated to accommodate the fluid reaction w σ to be placed, in which case the fluid reaction mixture is always in each case Only the bad-holes flow into each chamber. This example further increases the number of amounts of the components used in the fluid reaction. In another preferred embodiment, two or more sampling tubes are provided, and the sampling tubes are each connected to the sleeve in a fixed manner in such a manner that each of the sampling S holes is directly disposed on the sleeve. Perforated, and individual sampling tubes are in the gap; ^ different south degrees open. In addition, the sleeve itself can be configured as a sampling tube by providing a perforation only at a point where there is a direct connection with a sampling tube in each case, and additionally in the sleeve A single additional perforation is provided at the n-point, and the fluid reaction mixture flows in through the perforations. Thus, the method and apparatus according to the present invention makes it possible to utilize an available factory analytical instrument in a simple manner to obtain an accurate knowledge of the actual reaction event and the true temperature, preferably also the temperature critical to the hot spot. In this way, operation which is substantially closer to the load limit of the catalyst is allowed; therefore, the catalyst' can be better utilized while at the same time preventing damage caused by poorly formed hot spots. In addition, based on the knowledge of actual reaction events, the catalyst activity can be spatially configured within the gap to match the manner in which the actual reaction event changes. In this way, the catalyst is protected, in particular in the region of more thermal stress, and thus its aging is better adjusted for the purpose of longer or more advantageous utilization. This can have a positive effect on the overall selectivity of the reaction in which the other reactor can operate substantially more uniformly. 97923.doc • 20·1376267. In addition, the adaptation of the catalyst to actual reaction events allows for the reduction of the required amount of heat carrier. The invention will be described in detail below with reference to the drawings. [Embodiment] Fig. 1 shows an illustration of a section of a reactor 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 disposed within the gap 2 and seals, for example, the thermal element 4 having four measuring points. The sleeve 3 and the heat element 4 protrude beyond the reactor through nozzles in the reactor jacket. The cross section of Figure 1 illustrates the cylindrical geometry of the sleeve 3 having the thermal element 4 disposed therein. The illustration in Fig. 2 illustrates the wearing surface of the reactor in the longitudinal direction in the region of the gap 2 between the two hot plates (not shown). In the gap 2, a sleeve 3 having a heat element 4 is placed at its transverse boundary 6 and an insulating element 5 is provided between the sleeve 3 and the lateral boundary of the gap 2. The cross section in Fig. 2 illustrates the hot plate 丨 (including its fixation to the lateral boundary 6), and the cylindrical design of the sleeve 3 having the thermal element 4 and the shape of the insulating member 5 are suitably designed. Figure 3 shows an illustration of a transverse plane of another embodiment in which the sleeve 3 of the thermal element 4 is horizontally aligned within the gap 2. The sleeve has perforations 7 near its end projecting into the gap, by which a sample of the reaction mixture can be taken. The illustration in Figure 4 illustrates a longitudinal section of another embodiment having a sleeve 3 having a perforation 7 in the sleeve 3 for taking the sample into the sampling tube 8 with a sampling tube 8 The sleeve 3 protrudes beyond the nozzle 9 and protrudes outside the counter 97923.doc-21- 1376267. The cross section in Fig. 4A illustrates an embodiment in which the sleeve 3 having the holes 7 and the sampling tube 8 is illustrated in cross section. Figure 5 shows an illustration of a cross section of a reactor having parallel hot plates 1 and intermediate gaps 2. The sleeve 3, which is illustrated by way of example, is shown and protrudes in its longitudinal direction into the gap 2 between the two hot plates 1, and the sleeve is opened outside the reactor by the nozzles 9 in the reactor jacket. Figure 6 shows the distribution of two preferred weld points on the surface of the hot plate: in each case, it illustrates a hot plate corresponding to 5 times the separation of the weld points on the horizontal axis and 5 times the column resolution on the vertical axis. The rectangular surface section of the crucible. The upper portion of Figure 6 illustrates a preferred weld spot distribution having a total of 33 weld points on the illustrated surface section of the hot plate having 5 times the weld separation and 5 times the column resolution, and The lower description shows another preferred arrangement having 25 solder joints on the surface of the surface. BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 shows a cross section of a reactor having a hot plate having a sleeve disposed therein for accommodating the center of the heat element, and a cross-sectional view in Fig. 1A. Figure 2 shows a carrier surface of another embodiment having a laterally disposed sleeve in a longitudinal section, a cross-sectional view in Figure 2A, and a sleeve white having a horizontal placement in the gap in the longitudinal section. A cross-sectional illustration in FIG. 3A and a detailed description in FIG. 3B. FIG. 4 shows a cross section of another embodiment having a sleeve f having a perforation and a sampling tube in the longitudinal wear surface, and FIG. 4A is a cross-sectional view. Illustrative, '97323.doc -22- 1376267 Figure 5 shows an illustration of the placement of the inventive sleeve within the hot plate module, and Figure 6 shows an illustration of the preferred weld spot distribution on the surface of the hot plate. In the figures, the same reference numerals indicate the same or corresponding features. [Main component symbol description] 1 Hot plate 2 Clearance 3 Sleeve 4 Heat element 5 Insulation element 6 Transverse boundary 7 Perforation 8 Sampling tube 9 Nozzle 97923.doc -23·

Claims (1)

1376^----- γΑ” El 修正畚換I 十、申請專利範圍: 第093138975號專利申請案 ’ 中文申請專利範圍替換本(丨⑼年丨〗月) 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—流體反應混合物之反應之方法,該反 應:具有垂直且彼此平行排列、同時在每_情況下均留 1隙(2)之兩個或兩個以上熱板⑴,肖異質微粒催化 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⑺,該方法包括選擇—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(2) 内於刀佈在每_間隙⑺之高度上的—或多個量測點處量 測。 2·如請求項1之方法,其中將一或多個間隙⑺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, 且該且合物係於分佈在每_間隙⑺之高度上的—或多個 量測點處測定。 3·種用於進行如凊求項1之方法之設備,其特徵為一套筒 (3) 4套筒係安置於該間隙(2)内且在該反應器外部打 開’且在海一情況下均密封-具有-或多個量測點之溫 度量測插件(4)。 4·如明求項3之设備,其中該套筒係在縱向上設置於該間隙 (2)内。 5. 如請求項3或4之設備, 其中該等熱板(1)係安置於: ,其各由彼此平行排列、 間隙(2)之兩個或兩個以上 • 一或多個立方形熱板模組内 同時在每一情況下均留有一 矩形熱板(1)形成, 97923-1001130,doc 1376267 6. 7. 8. 9. 10. 月々洵修正替換頁 -該等熱板模組完全由一釋放壓力之主要為圓柱形的外 殼所包圍’該外殼包括一圓筒夾套及蓋,其在兩個末 端處封閉該外殼,且其縱轴經對準成平行於該等熱板(1) 之平面, -將一或多個密封元件以使該流體反應混合物除了流過 由該等蓋所界限之反應器内部外僅流過該等間隙(2)之 方式設置,及 -具有一或多個相互獨立之溫度量測插件(4)之每一熱板 模組較佳配備有兩個或三個、更佳為三個溫度量測插 件(4) 〇 如請求項3或4之設備,其中該溫度量測插件(4)為一多重 量測插件 如請求項3或4之設備,其中該套筒為一金屬管,該套筒 尤其具有一在4至15毫米範圍内之外徑,且具有〇8至15 毫米之壁厚度。 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。 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—相對較小之分離度, :在其餘反應器區域内彼此間具有一相對較大之分離 度0 如請求項3或4之設備 ” 狁封該溫度量測插件(4)之該 套疴(3)在該反應器上方與 万以如下方式打開:可使較 97923-1001l30.doc 佳配備有等距量測點之該溫度量測插件(4)在該套筒(3) 内連續地移位,以用於不間斷地量測溫度分佈。 11. 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。 12. 如請求項丨丨之設備,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 11寸之外棱及4毫米或5/32英**寸之内徑。 13. 如請求項11之設備,其中該溫度量測插件(4)具有4〇個量 測點及約2.5毫米之外徑,且該套筒(3)具有5毫米或3/16 英吋之外徑及3毫米或1/8英吋之内徑。 14. 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。 15·如請求項4之設備,其中該套筒(3)係設置於該間隙(?)之 橫向邊界(6)處。 16.如請求項15之設備,其中在該間隙(2)之該橫向邊界(6)與 該套筒(3)之間設置一絕緣元件。 1 7_如β求項3之没備,其中該套筒(3)係水平地設置於該間隙 (2)内。 18. -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, 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中之至少一取樣管該取 樣管係以如下方式設置於該套筒(3)内:該流體反應混合 物流過該套筒(3)内之該等穿孔(7)而進入該取樣管(8) 97923-100H30.doc 1376267 " · . - — I _ · —— 中,且自該取樣管(8)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,且具有設置於其炎套表面上 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. 如晴求項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. 如凊求項22之设備’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。 25. 如請求項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(8)以如下方式以一固定方式各連接 至該套筒(3):每一取樣管(8)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 97923-1001130.doc 1376267 ,, 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) 〇 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。 97923-1001130.doc1376^----- γΑ” El Amendment I I. Patent Application: Patent Application No. 093138975 'Chinese Patent Application Substitution Replacement (丨(9)年丨月) for monitoring, control and/or A method of adjusting the reaction of a fluid reaction mixture in the presence of a heterogeneous particulate catalyst in a next reactor, the reaction: having two or two vertically and parallel to each other while leaving 1 gap (2) in each case More than one hot plate (1), a heterogeneous particulate catalyst is disposed in the gaps (2), and the fluid reaction mixture passes through the gaps (7), the method comprising selecting - or multiple temperatures as a monitoring, control and / or regulation The parameter 'the or the temperature system, measured in the - or a plurality of gaps (2) at the height of the knife cloth at the height of each gap (7) - or a plurality of measuring points. Where the composition of the fluid reaction mixture within one or more of the gaps (7) is selected as another monitoring, control and/or conditioning parameter and is distributed at a height of each gap (7) - or Determined at multiple measurement points. Apparatus for carrying out the method of claim 1, characterized in that a sleeve (3) 4 sleeve is placed in the gap (2) and opened outside the reactor 'and sealed in the case of the sea a temperature measuring insert (4) having - or a plurality of measuring points. 4. The apparatus of claim 3, wherein the sleeve is disposed in the gap (2) in the longitudinal direction. The apparatus of item 3 or 4, wherein the hot plates (1) are disposed in: each of which is arranged in parallel with each other, two or more of the gaps (2) • one or more cubic hot plate modules At the same time, in each case, there is a rectangular hot plate (1) formed, 97923-1001130, doc 1376267 6. 7. 8. 9. 10. 々洵 々洵 correction replacement page - these hot plate modules are completely released by a pressure Surrounded by a generally cylindrical outer casing, the outer casing includes a cylindrical jacket and a cover that encloses the outer casing at both ends with its longitudinal axis aligned parallel to the plane of the hot plates (1). - one or more sealing elements such that the fluid reaction mixture flows only outside the interior of the reactor bounded by the caps The gaps (2) are arranged, and each of the hot plate modules having one or more independent temperature measuring inserts (4) is preferably equipped with two or three, more preferably three temperatures. Measuring device (4), such as the device of claim 3 or 4, wherein the temperature measuring insert (4) is a multi-weight measuring insert such as the device of claim 3 or 4, wherein the sleeve is a metal tube, The sleeve has, in particular, an outer diameter in the range of 4 to 15 mm and a wall thickness of 8 to 15 mm. The apparatus of claim 3 or 4 wherein the sleeve (3) is inside the reactor Has one or more break points. The apparatus of claim 3 or 4 wherein the measuring points of the temperature measuring insert (4) are arranged to have each other within a reactor zone having a desired temperature limit and/or a particularly large temperature gradient - Relatively small resolution: a relatively large degree of separation between each other in the rest of the reactor zone. 0 Device of claim 3 or 4" Sealing the set of temperature measuring inserts (4) Above the reactor and open as follows: the temperature measuring insert (4) which is better equipped with equidistant measuring points than the 97923-1001l30.doc can be continuously displaced in the sleeve (3) For measuring the temperature distribution without interruption. 11. The device of claim 3 or 4, wherein the temperature measuring insert (4) has 5 to 6 measuring points. Apparatus, wherein the temperature measuring insert (4) has 2 measuring points and an outer diameter of about 3.8 mm, and the sleeve (3) has 6 mm or 1/4 inch 11 inch outer edge and 4 mm or The inner diameter of the 5/32 inch ** inch. 13. The device of claim 11, wherein the temperature measuring insert (4) has 4 measuring points and about 2.5 The outer diameter of the meter, and the sleeve (3) has an outer diameter of 5 mm or 3/16 inch and an inner diameter of 3 mm or 1/8 inch. 14. The device of claim 4, wherein the sleeve (3) is disposed in the gap (2) in the longitudinal direction. 15. The apparatus of claim 4, wherein the sleeve (3) is disposed at a lateral boundary (6) of the gap (?). The apparatus of claim 15, wherein an insulating member is disposed between the lateral boundary (6) of the gap (2) and the sleeve (3). The sleeve (3) is disposed horizontally within the gap (2). 18. A device for performing the method of claim 2, wherein the device is as defined in any one of claims 3 to 16. Outside the apparatus, in each case a sleeve (3) is provided in one or more gaps (2), and the sleeve has perforations (7) and at least one sampling tube for introduction into the sleeve The sampling tube is disposed in the sleeve (3) in such a manner that the fluid reaction mixture flows through the perforations (7) in the sleeve (3) and enters the sampling tube (8) 97923-100H30.doc 1376267 &quo t; · . - - I _ · -, and the fluid reaction mixture is removed from the sample tube (8) to the outside of the reactor and analyzed. 19. The apparatus of claim 18, Wherein the sampling tube (8) is attached to the sleeve (3) in a fixed manner in such a manner that one of the sampling tubes (8) is directly disposed on one of the perforations (7) of the sleeve (3) 20. The device of claim 18, wherein the sampling tube (8) is rotatably disposed within the perforated sleeve (3) and has a surface disposed on the surface of the sleeve that is offset as follows Two or more holes: The fluid reaction mixture always flows into the sampling tube (8) only through one of the holes. 21. The apparatus of claim 20, wherein the holes of the sampling tube (8) are designed as slots in their longitudinal direction. 22. The apparatus of claim 18, wherein each of the sampling tubes (8) has two or more mutually independent chambers each having a bore through which the fluid reaction mixture is The perforations (7) within 3) flow into the well and the fluid reaction mixture is removed from each chamber separately and analyzed. 23. The apparatus of claim 22 wherein the chambers are disposed adjacent to each other or concentrically. 24. The apparatus of claim 21, wherein the sampling tube (8) having a plurality of chambers is designed to be rotatable about its longitudinal axis. 25. The apparatus of claim 18, wherein two or more sampling tubes (8) are provided, and the sampling tubes (8) are each connected to the sleeve (3) in a fixed manner as follows: The hole of each sampling tube (8) is directly disposed on one of the perforations (7) of the sleeve (3), and the individual sampling tubes (8) are respectively 97923-1001130.doc in the gap (2) 1376267 ,, opened at a different height. 26. The apparatus of claim 18, wherein the sleeve (3) itself is designed as a sampling tube (8) 〇 27. A method for incorporating the apparatus of claim 3 into a reactor, wherein The apparatus is disposed from the same side of the reactor as the feed side of the fluid reaction mixture. 28. The method of claim 27, wherein the apparatus 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 is a perforation (7) in the upper region, especially near the midpoint of the gap (2). 29. The method of claim 27, wherein the apparatus is disposed, 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 The plate (1) is subjected to partial or complete evaporation of the heat carrier under the reaction conditions. 97923-1001130.doc 97923-fig-10K)625,doc 137626797923-fig-10K) 625, doc 1376267 圖ΙΑ 97923-fig-1010625.doc 1376267 ,. (ahA日料铮換頁·Figure 923 97923-fig-1010625.doc 1376267 ,. (ahA 铮 铮 铮 圖2 97923-fig-1010625.doc 1376267Figure 2 97923-fig-1010625.doc 1376267 圖2Α 97923-fig-1010625.doc -4 1376267Figure 2Α 97923-fig-1010625.doc -4 1376267 97923-fig-1010625.doc97923-fig-1010625.doc 1376267 |^\年1 W日修正替換育1376267 |^\year 1 W day correction replacement education 圖3A 97923-fig-1010625.doc 6-Figure 3A 97923-fig-1010625.doc 6- B 3 圖 97923-fig-1010625.doc 1376267B 3 Figure 97923-fig-1010625.doc 1376267 3 圖4 97923-fig-1010625.doc3 Figure 4 97923-fig-1010625.doc 97923-flg-1010625.doc -9- 1376267 Μ V. Π ι97923-flg-1010625.doc -9- 1376267 Μ V. Π ι 〇〇 ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο 0 0〇〇0 οι〇〇〇 _ ρ〇〇Ο Ο^0^0 ο ο ο ο .c ^ ο ο ο ο ο 97923-fig-1010625.doc • 10- 1376267 产一— C? -ι/0 : - cp- 〇 -e- 〇 -e- 〇 -e- 〇 -e- 〇 广、 o 〇 〇 〇 〇 〇 〇 〇 〇 o o o -e- 〇 -Θ- 〇 -e- 〇 〇 -Θ- o o 0 〇 〇 〇 〇 〇 〇 〇 〇 〇 〆 〇 0 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 圖6 97923-fig-1010625.doc〇〇ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο ο 97923-fig-1010625.doc • 10- 1376267 产一— C? -ι/0 : - cp- 〇-e- 〇-e- 〇-e- 〇-e- 〇广, o 〇〇〇 〇〇〇〇〇ooo -e- 〇-Θ- 〇-e- 〇〇-Θ- oo 0 〇〇〇〇〇〇〇〇〇〆〇0 〇〇〇〇〇〇〇〇〇〇〇〇〇〇 Figure 6 97923-fig-1010625.doc
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DE102009047291A1 (en) 2009-11-30 2010-09-23 Basf Se Producing (meth)acrolein, by heterogeneous catalyzed gas phase-partial oxidation, comprises guiding reaction gas mixture through a fresh fixed catalyst bed present in a reactor at increased temperature
DE102011076931A1 (en) 2011-06-03 2012-12-06 Basf Se Aqueous solution containing acrylic acid and its conjugate base
DE102020007213A1 (en) 2019-12-17 2021-06-17 Silica Verfahrenstechnik Gmbh Method and device for treating a gas contaminated with harmful and / or useful components

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