201034954 六、發明說明： 【發明所屬之技術領域】 本發明關於使四氯矽烷與氫反應而轉化成三氯矽烷的 三氯矽烷製造裝置，尤其關於不易發生熱膨脹所致的變形 或破損，三氯矽烷的回收效率優異，且轉化效率亦優異的 三氯矽烷製造裝置。 【先前技術】 三氯矽烷（SiHCh)係半導體、液晶面板、太陽電池等之 〇 製造時所使用的特殊材料氣體。近年來，需求係順利地擴 大，作爲電子領域所廣泛使用的CVD材料，今後亦期待成 長。 三氯矽烷係藉由使四氯矽烷（SiCl4)與氫（H2)接觸，達成 以下的熱平衡狀態而生成。201034954 VI. TECHNOLOGICAL FIELD OF THE INVENTION [Technical Field] The present invention relates to a device for producing triclosan which converts tetrachloromethane with hydrogen to convert it to trichloromethane, and more particularly to deformation or breakage caused by thermal expansion, trichloro A device for producing triclosan having excellent recovery efficiency of decane and excellent conversion efficiency. [Prior Art] A special material gas used in the manufacture of a trichlorosilane (SiHCh)-based semiconductor, a liquid crystal panel, a solar cell, or the like. In recent years, demand has been rapidly expanded, and CVD materials widely used in the electronics field are expected to grow in the future. Trichloromethane is produced by bringing tetrachloromethane (SiCl4) into contact with hydrogen (H2) to achieve the following thermal equilibrium state.
SiCl4 + H2〇 SiHCl3 + HC1 (1) 此反應係藉由在反應容器中將由已氣化的四氯矽烷與 氫所構成的原料氣體加熱到800 °C〜1300 °C而進行。 Ο 於由反應容器所排出的高溫反應生成氣體中，除了所 生成的三氯矽烷及氯化氫，亦含有大量未反應的四氯矽院 及氫。爲了由反應生成氣體中取出三氯矽烷，使用一種利 用四氯矽烷與三氯矽烷之沸點的不同，以蒸餾塔來凝縮的 方法。具體地’於冷凝器中’分成凝縮份的氯矽烷與未凝 縮份的氯化氫、氫、未凝縮氯矽院，再藉由深冷分離而冷 卻到-70 °C左右爲止，以由凝縮份中分離出三氯矽烷。 於由反應生成氣體中分離出目的之三氯矽烷時，若將 -4- 201034954 由反應容器所剛導出的高溫之反應生成氣體突然地導入蒸 餾塔，則對蒸餾塔會有施加過度的負荷，故典型地於將反 應生成氣體導入蒸餾塔之前，必須先在急冷塔中預備地冷 卻。 然而，即使所謂的預備冷卻，若冷卻力不十分，則平 衡傾向於四氯矽烷側，所生成的三氯矽烷就得再度返回四 氯矽烷。因此，爲了謀求三氯矽烷的回收效率之提高，於 平衡充分達到三氯矽烷側的時間點，必須盡可能地瞬間將 〇 反應生成氣體冷卻到指定溫度爲止而凍結平衡。爲了瞬間 凍結上述平衡狀態，典型地必須在1秒以內將反應生成氣 體急冷到600C左右爲止。 作爲具備使四氯矽烷與氫反應而轉化成三氯矽烷，再 將反應生成氣體冷卻的機構之反應容器，例如有專利文獻 1中記載者。若依照此文獻所記載的反應器，於反應器的 底部連接有熱交換器，將在熱交換器中預熱的由氫與氯矽 烷所成的原料氣體供應給反應器。所供給的原料氣體係在 © 反應器內所設置的外室向上前進，此時被反應器內設置的 發熱體所加熱。加熱所生成的氣體係藉由設置於反應器的 上部的轉向器改變進行方向，在反應器內的內室向底部前 進’再流入熱交換器，於熱交換器中，由經加熱的反應生 成氣體往供應給反應器內的原料氣體進行熱的交接。藉此 ，反應生成氣體被冷卻，原料氣體被預備加熱。 再者作爲另一例，有專利文獻2中記載者。此文獻中 提案一種三氯矽烷製造裝置，其具備將含四氯矽烷與氫的 201034954 供給氣體供應給內部而生成含三氯矽烷與氯化氫的反應生 成氣體之反應容器，將反應容器的內部加熱之加熱機構’ 收納反應容器及加熱機構的收容容器’對反應容器內供應 供給氣體的氣體供給內筒，在氣體供給內筒的外側大致同 軸配置的氣體供給內筒之外周面與自己之內周面之間形成 反應生成氣體的排氣流路之氣體排氣外筒’以及在內側支 持氣體排氣外筒且在內部形成有使冷媒流通的冷媒路之冷 卻筒。於此三氯矽烷製造裝置中’高溫狀態的反應生成氣 〇 體在排氣流路流動而排出之際’藉由在氣體排氣外筒的外 側所設置的冷卻筒流動的冷媒而使由外側冷卻的同時’使 在氣體排氣外筒的內側所設置的氣體供給內筒向反應容器 內部，與流入的供給氣體進行熱交換而冷卻。即’藉由從 氣體排氣外筒的內外來同時地冷卻，以謀求冷卻效率的提 高。 然而，於專利文獻1所記載的反應器中，反應生成氣 體的冷卻係僅任憑在與鄰接行進的原料氣體之熱交換’故 〇 瞬間地將達到1 000°C以上的反應生成氣體冷卻到600°c左 右爲止係困難。因此，於到排出反應生成氣體爲止之間， 上述平衡徐徐地傾向四氯矽烷側，而損失好不容易生成的 三氯矽烷之一部分。又，於專利文獻2所記載的裝置中， 雖然設有在氣體排氣外筒的周圍形成有冷媒路的冷卻筒， 但是於此情況下，由於反應生成氣體的冷卻係經由氣體排 氣外筒的內壁及外壁委以熱交換，故在冷卻速度及能力之 點未必能說是充分。 -6- 201034954 再者，於專利文獻2記載的裝置中，反應容器的底部 係被下部支持圓板所封閉，而且由於此下部支持圓板係僅 在其中央部被由構成收容容器的底板之底部支持構件的中 央向上的突出之支持柱構件所支撐，故即使構成反應容器 的反應筒壁進行熱膨脹，下部支持圓板係可以支持柱構件 爲中心而撓曲變形，可吸收其應力。然而，儘管於反應容 器的上部配置高溫的反應生成氣體所通過的氣體排氣外筒 或氣體排氣管，但是反應容器的上部係藉由上部支持圓板 〇 與氣體供給內筒及上部圓環板與氣體排氣外筒而與收容容 器接觸，被支持·固定。即，高溫氣體所流動氣體排氣外 筒及氣體排氣管，由於被收容容器、頂板部、冷卻筒、供 給氣體導入部等所支持•固定，故無法緩和構件的熱膨脹 所致的應力集中，容易導致變形或破損。又，由於在氣體 排氣外筒的外側，低溫的冷卻筒係鄰接而設置，若過度提 高冷卻能力，則在構成該部位的各構件發生局部過度的溫 度差，有由應力的集中而導致破損之虞。 〇 因此，作爲比如此經由排氣管的內壁或外壁的冷卻方 法來更強力且瞬間地冷卻反應生成氣體之方法，有提案將 反應生成氣體由高溫的反應容器導出到急冷塔，在其中使 冷卻液直接接觸反應生成氣體，利用冷卻液氣化之際的蒸 發潛熱由反應生成氣體中奪取熱之方法。 例如專利文獻3中提案一種裝置，其具備藉由將四氯 矽烷與氫導入反應室，使在60(TC〜120(TC的溫度進行轉 化反應，而得到含有三氯矽烷與氯化氫的反應生成氣體後 -7- 201034954 ，藉由對由反應室所導出的反應生成氣體，噴灑經冷卻到 室溫的氯矽烷混合物而使接觸，在1秒以內冷卻到3〇〇°c 以下爲止的冷卻手段。 [專利文獻1]特開平6-293511號公報 [專利文獻2]特開2008- 1 3 3 1 7 5號公報 [專利文獻3]特公昭57-3 8524號公報 【發明內容】 還有，於專利文獻3記載的裝置中，反應爐與急冷塔 〇 係經由急冷塔之側方所設置的連接管來連接，在連接管與 反應爐的接合部形成封閉的端部。而且，使探針貫穿此封 閉的端部，經過該探針將反應爐所生成的反應氣體導出到 急冷室。 然而，達到高溫的反應爐與低溫的急冷室，由於被連 接管與反應爐的接合部之封閉的端部壁面所遮蔽，故在遮 蔽急冷塔與反應爐的端部壁面與其附近傍發生局部的大溫 度差。結果，熱膨脹所致的應力集中於該部位，而會發生 〇 變形或破損。又，貫穿端部壁面而固定的探針亦熱膨脹， 應力集中於探針與端部壁面的接合部，而會發生變形或破 損。 即，於對反應生成氣體直接噴吹冷卻液而瞬間冷卻的 系統中，急冷效率優異，但另一方面，由於裝置中有局部 的大溫度差，故如何避免熱膨脹所致的應力集中係成爲問 題。儘管如此，專利文獻3中完全沒有觸及用於吸收或緩 和該應力的手段。 201034954 本發明係鑒於上述情事而完成者，目的爲提供一種三 氯矽烷製造裝置，其不易發生熱膨脹所致的變形或破損， 三氯矽烷的回收效率優異，而且三氯矽烷的轉化效率亦優 異。 本發明爲了解決前述問題，採用以下的構成。即，本 發明的三氯矽烷製造裝置之特徵爲具備： 具備由含四氯矽烷與氫的原料氣體來生成含三氯矽烷與 氯化氫的反應生成氣體之大略圓筒狀的反應容器、加熱前 〇 述反應容器的加熱器、及收納前述反應容器和加熱器且與 前述反應容器僅以反應容器之底部接觸的外筒容器之反應 爐， 將前述反應生成氣體冷卻之急冷塔， 在前述反應爐與急冷塔之間連結的連結筒， 以通過在前述反應容器的外周面所大略垂直地連接之前 述連結筒內部而到達前述急冷塔的方式所配置的由反應爐 中將前述反應生成氣體導出到急冷塔之抽出管，及 〇 在前述連結筒內部以覆蓋前述抽出管的方式大略同軸地 配置，一端接合於連結筒的內周，另一端接合於抽出管的 外周之波紋管。 <防止熱膨脹所致的破損> 於本發明的此三氯矽烷製造裝置中，反應容器係於僅 其底部與外筒容器的底部接觸之狀態下被安定地收納在反 應爐內。此處，反應容器係在其外周面連接抽出管的一端 ，由於抽出管係在連結筒的內部以可伸縮的波紋管來保持 201034954 ，故不會實質上貢獻反應容器的固定，亦不會對反應容器 施加過度的推壓力。即，反應容器係於僅其底部與外筒容 器接觸的狀態下被收納在外筒容器內，而且不用任何固定 手段，由於只不過藉由其自重而安定地固定在外筒容器底 部，即使發生加熱所致的熱膨脹，也不會導致應力的集中 〇 又，抽出管由於藉由在連結筒內於抽出管與連結筒之 間與此等大致同軸配置的波紋管而保持伸縮自在，故即使 〇 由於反應生成氣體的通過而被加熱進行熱膨脹，也可藉由 波紋管追隨其而伸縮，避免應力的集中。 然而，藉由以波紋管來伸縮自在地保持抽出管的一端 ，同時成爲反應容器係在其底部僅由自重來支撐的構成， 波紋管不僅對於抽出管的熱膨脹，而且對於反應容器的熱 膨脹亦可追隨而變形。因此，即使對於反應容器及抽出管 兩方的熱膨脹，也可適宜變形而吸收應力，可保護裝置全 體防止變形或破損。 〇 又，波紋管亦兼具作爲遮斷反應爐內部的空間與急冷 塔內部的空間之遮斷構件的任務，由於可自在地變形，故 可更安定地維持兩塔間的氣密狀態。 還有，於此三氯矽烷製造裝置中，爲了將在反應爐內 的反應容器所生成的反應生成氣體，經由在反應容器的外 周面所大略垂直連接之抽出管而導出到急冷塔，故可在從 反應容器到急冷塔爲止以直線的最短距離來連繋。因此， 抽出管可爲大略直線狀的中空管，由於不需要成爲複雜的 -10- 201034954 形狀，故耐熱強度亦優異。即，於以波紋管來保持抽出管 的情況中，當抽出管彎曲時，由於波紋管的伸縮強度等， 也很有可能反而在抽出管的彎曲部或與反應容器的連續部 負載大的應力，但於此三氯矽烷製造裝置中，由於抽出管 爲單純的大略直線狀，在抽出管亦不會負載局部過度的應 力。 再者，由於波紋管在連結筒內部以覆蓋抽出管的方式 而配置，故可在該區域內形成兩空間之中間溫度區域。即 〇 ，在連結筒內，形成從外筒容器側到急冷塔側平緩下降的 中間溫度區域，可分散對抽出管所施加熱負荷。因此，可 防止在抽出管發生局部的大應力。 如此地，藉由以波紋管來伸縮自在地保持抽出管的一 端，同時成爲反應容器係在其底部僅由自重來支撐的構成 ，暴露於高溫中的反應容器及抽出管皆自由地膨脹或收縮 ，可避免應力的集中，可保護裝置全體防止變形或破損。 <回收效率的提高> © 如上述地，本發明的三氯矽烷製造裝置’由於對於應 力的發生具有極優異的耐性，故可與冷卻效率高的急冷系 統倂用。因此，例如在急冷塔的內部對所取入的反應生成 氣體直接噴灑冷卻液，利用冷卻液氣化之際的蒸發潛熱來 瞬間地奪取熱之類型的急冷系統亦特別適合。於此情況下 ，由於利用冷卻液之氣化所伴隨的蒸發潛熱’與通過形成 反應生成氣體的排氣流路之壁而使與冷媒或供給氣體進行 熱交換的情況相比，可遠更高效率地且經濟地進行冷卻。 -11- 201034954 又’藉由以對反應容器的外周面大略垂直地連接抽出 管’照原樣直線地到達急冷塔之方式來配置，可使從反應 容器到急冷塔爲止的距離成爲最小限度。因此，於平衡傾 向於三氯矽烷側的狀態下短時間內可供應給急冷塔，可減 低反應生成氣體在流經抽出管之間被冷卻而損失的三氯矽 烷量。 再者’藉由成爲如此的構成，由於抽出管係大略水平 地插入急冷塔’故反應生成氣體亦同樣大略水平地噴出。 〇 一般地，於對反應生成氣體噴灑冷卻液的方法中，使用從 急冷塔的上方向下方噴灑冷卻液，將由於重力而積存在急 冷塔的下部之冷卻液送到冷卻裝置進行冷卻後，用泵送往 冷卻塔上部，而再度供噴灑的循環系統。於此三氯矽烷製 造裝置中，當從冷卻塔的上方向下方噴灑冷卻液時，由於 可使反應生成氣體大略水平地噴出，故可使反應生成氣體 與冷卻液大略垂直地衝撞。結果可確實地混合兩者，可高 效率地進行冷卻。又，由於相對於抽出管的軸向而言，冷 〇 卻液的噴灑方向係成爲大略垂直，故所噴灑的冷卻液液流 入抽出管的內部之虞係低，亦可保護抽出管或反應容器的 內部防止腐蝕。 如此地，由於可瞬間高效率地冷卻平衡傾向於三氯矽 烷的狀態之反應生成氣體’故可大幅改善三氯矽烷的回收 效率。 <轉化效率的提高> 又，由於上述式（1)之由四氯矽烷及氫生成三氯矽烷的 -12- 201034954 反應係吸熱反應，爲了提高三氯矽烷的轉化效率，必須至 少使反應容器內部的熱不往外逃。 於本發明的三氯矽烷製造裝置中，由於進行三氯矽烷 的轉化反應之反應容器係僅在反應容器底部與外筒容器接 觸，故可壓低反應容器與外筒容器的接觸面積。結果，可 抑制熱由反應容器往外筒容器的傳達，可抑制熱往外部逃 。因此，可提供由四氯矽烷往三氯矽烷的轉化效率。 如此地，若依照本發明的三氯矽烷製造裝置，藉由以 〇 波紋管來伸縮自在地保持抽出管的一端，同時成爲反應容 器係在其底部僅由自重來支撐的構成，反應容器及抽出管 係自由地膨脹或收縮而可避免應力集中，可保護裝置全體 防止變形或破損。 因此，隨著該耐熱性提高，與冷卻效率高的急冷系統 倂用係成爲可能，可不損傷設備而比以往遠高效率地回收 三氯矽烷。再者’藉由成爲上述構成，由於可抑制熱從反 應容器往外部的洩漏，故可提高三氯矽烷的轉化效率。 〇 如此地，藉由同時地提高上述耐熱安定性、回收效率 及轉化效率，可改善三氯矽烷的生產性。 【實施方式】 以下，使用圖式來說明本發明的實施形態。尙且，於 所有的圖式中，同樣的構成要素附有同一符號，適宜地省 大略說明。 第1圖係示意地顯示本發明的三氯矽烷製造裝置之一 實施形態。又，第2圖係示意地顯示該三氯矽烷製造裝置 -13- 201034954 的連結筒周邊之剖面。 本實施形態的三氯矽烷製造裝置係如第1圖及第2圖 所示地，具備： 具備由含四氯矽烷與氫的原料氣體來生成含三氯矽烷與 氯化氫的反應生成氣體之大略圓筒狀的反應容器10、加熱 前述反應容器10的加熱器11、收納前述反應容器10及加 熱器11且與前述反應容器10僅以反應容器10之底部接 觸的外筒容器12之反應爐1， 〇 將前述反應生成氣體冷卻之急冷塔4， 在前述反應爐1與急冷塔4之間連結的連結筒3， 以通過前述反應容器10的外周面所大略垂直地連接之 前述連結筒3內部而到達前述急冷塔4的方式所配置的由 反應爐1中將前述反應生成氣體導出到急冷塔4之抽出管 2，及 在前述連結筒3內部以覆蓋前述抽出管2的方式大略同 軸地配置，一端接合於連結筒3的內周，另一端接合於抽 Ο 出管2的外周之波紋管30。 <反應爐> 反應爐1具備反應容器10、以包圍該反應容器10的外 側之方式所配置的長條狀加熱器11、收納前述反應容器 10及加熱器11的外筒容器12。藉由於經絕熱的外筒容器 12內部以加熱器11來加熱反應容器1〇的外壁’將反應容 器10內部保持在約8 00°C至約1 300°c的高溫’使由反應 容器10的底部所設置的原料氣體導入口 13所供給的四氯 -14- 201034954 矽烷與氫之混合氣體在反應容器10內部反應，而生成含 三氯矽烷與氯化氫的反應生成氣體。 <反應容器> 反應容器10係用於使四氯矽烷與氫在高溫環境下反應 的大略圓筒形狀之容器，具有用於取入原料氣體的原料氣 體導入口 13、與連接於後述抽出管2之用於導出反應生成 氣體的反應生成氣體抽出口 14。於本實施形態中，原料氣 體導入口 13係設置在反應容器10的底部中央，反應生成 〇 氣體抽出口 14係設置在反應容器10的上方之外周面。 原料氣體導入口 13係開口的周圍自底部大略垂直地延 伸而形成管狀突出部19，成爲嵌合於後述外筒容器12底 部所設置的原料氣體導入開口部17之構成。 較佳爲反應容器10的內周面及/或外周面係經碳化矽被 膜處理。碳化矽被膜由於對於化學分解具有極高的耐性， 故可防止碳組織的化學浸蝕。因此，藉由施予碳化矽被膜 處理，可保護反應容器10的表面防止腐蝕。 〇 〈加熱器〉 加熱器11具備在上下方向延伸的複數之長條狀碳製發 熱體15、與連接於該發熱體15之一端的用於供應電力給 發熱體15的電極16。加熱器11係以複數圍繞反應容器 10的周圍之方式所配置，藉由控制供給電力量而從反應容 器1〇的外側來調節反應容器10內部的溫度。 <外筒容器> 外筒容器1 2係外側由不銹鋼等的金屬所構成，內側經 -15- 201034954 碳板、耐火磚、絕熱磚等的絕熱材所被覆的大略圓筒形狀 之容器。外筒容器12係收納前述反應容器10及前述加熱 器11，使彼等與外界絕熱。於外筒容器12中，將反應容 器10收納之際，在對應於其原料氣體導入口 13及反應生 成氣體抽出口 14的位置分別設置原料氣體導入開口部17 及反應生成氣體抽出開口部18。在反應生成氣體抽出開口 部18設有凸緣等的接合手段，而成爲與後述的連結筒3 可能連接。 〇 原料氣體導入開口部17係在上述反應容器10的底部 嵌合一形成有當作原料氣體導入口 13的管狀突出部19嵌 合，其口徑與管狀突出部19的外徑大致相同。 於在外筒容器12中收納反應容器10之際，藉由在外 筒容器12底部所設置的原料氣體導入開口部17,嵌合反 應容器10的底部所設置的管狀突出部19，而以確保反應 容器10原料氣體的流入路之方式來定位，同時藉由反應 容器10的自重而安定地固定在外筒容器12的底部。 〇 〈連結筒〉 連結筒3係在一端具有連接於反應爐1的接合手段， 在另一端具有連接於急冷塔4的接合手段。本實施形態的 連結筒3係由不銹鋼等的金屬所構成，如第2圖所示地， 在一端具有可連接於外筒容器12的反應生成氣體抽出開 口部18之凸緣’在另一端具有用於連接於後述急冷塔4 的反應生成氣體導入開口部42之凸緣。 〈急冷塔> -16· 201034954 急冷塔4具備圓筒狀的金屬製容器40、對該容器內所 設置的容器內噴灑冷卻液的噴嘴41、取出前述容器的底部 所積存的冷卻液而使循環到噴嘴41的泵（省大略圖示）、用 於將冷卻液冷卻的冷卻裝置（省大略圖示）、與用於由急冷 塔4頂部取出冷卻後的反應生成氣體之導管（省大略圖示） 。在急冷塔4的側壁設有用於連接前述連結筒3的反應生 成氣體導入開口部42，在該反應生成氣體導入開口部42 設有用於與連結筒3連接的凸緣等接合手段。噴嘴41係 〇 以能向導入急冷塔4的反應生成氣體，由上方向下方噴灑 冷卻液的方式，設置在反應生成氣體導入開口部42的上 部附近。 用於反應生成氣體之冷卻的冷卻液，例如由三氯矽烷 與四氯矽烷的混合液所構成，相對於四氯矽烷與三氯矽烷 的全體量而言’，四氯矽烷的比可爲1〜0.5。溫度較佳爲60 °C以下。例如，較佳爲使用四氯矽烷：三氯矽烷的組成比係 85:15、溫度係40°C左右者。 Ο 由急冷塔4的頂部所取出的冷卻後之反應生成氣體係 經由導管再送到蒸餾塔，而進行目的之三氯矽烷的分離。 <抽出管> 抽出管2係通過連結筒3內部而連繫反應容器10內部 與急冷塔4內部的碳製管狀構件，將反應容器10內的反 應生成氣體導出到急冷塔4。 構成抽出管2的材質係氣密性優異的石墨材，特別地 從由於微粒子構造而強度高、熱膨脹等特性對於任一方向 -17- 201034954 皆相同來看，較佳爲使用耐熱性及耐蝕性亦優異的等方向 性高純度石墨。 特別地，較佳爲抽出管2的內周面及/或外周面係經碳 化矽被膜處理，該碳化矽被膜係藉由CVD法以10〜500μπι 的厚度所形成。碳化矽被膜由於對於化學分解具有極高耐 性，故可防止碳組織的化學浸鈾。因此，藉由施予碳化矽 被膜處理，可保護抽出管2的表面防止腐蝕。 本實施形態的抽出管2係由複數的構件所構成，在將 〇 裝置組裝之際，係由主要位於反應爐1內的第一構件21、 主要位於連結筒3內的第二構件22及主要位於冷卻塔內 的第三構件23所構成。即，第一構件21係在一端具有與 反應容器10的反應生成氣體抽出口 14之連接部，在另一 端具有用於連結第二構件22的接合手段，第二構件22係 在兩端具有用於連結第一構件21或第三構件23的接合手 段，第三構件23係在一端具有用於連結第二構件22的接 合手段，在另一端具有反應生成氣體噴出部24。 〇 抽出管2的接合手段係以接合後述的波紋管30之方式 ，在抽出管2的外周側形成突出部2 5。作爲形成如此突出 部25的接合手段，典型地可使用凸緣。又，亦可使用大 略圓筒狀的管狀構件，由外側以環來螺合締結對接的端部 。於此情況下，環係形成用於固定波紋管30的突出部25 〇 <波紋管> 波紋管3 0係由金屬所構成的波紋構造之構件，在軸心 -18- 201034954 方向可伸縮，同時在徑向亦可變形。波紋管30係可爲金 屬製，更佳爲不銹鋼鋼製，可爲沃斯田鐵系不銹鋼鋼製或 肥粒鐵系不銹鋼鋼製。 波紋管30較佳爲山的高度係入口徑的2〜10%右右， 山與山之間隔係全長的2〜8%左右。再者，較佳爲軸向的 位移量係入口徑的3〜10%，與軸垂直方向的位移量係全長 的2〜5%左右。又，山的間隔或高度可爲均一或不均一。 波紋管30係在連結筒3內部以覆蓋抽出管2的外側之 〇 方式大致同軸配置，一端接合於連結筒3的內周，另一端 接合於抽出管2的外周。 於本實施形態中，波紋管30與連結筒3內周之連接， 係藉由在外筒容器12的反應生成氣體抽出開口部18所設 置的接合手段與在連結筒3所設置的接合手段之間夾入甜 甜圈狀的板材31，在該板材31之伸出連結筒3內的部分 固定波紋管30的一端而進行。又，波紋管30與抽出管2 外周的連接，係藉由在構成抽出管2的第二構件22與第 〇 三構件23之連結所使用的凸緣固定波紋管30的一端而進 行。 波紋管30係伸縮自在地保持抽出管2，同時氣密地遮 斷反應爐1內部的高溫空間與急冷塔4內部的低溫空間。 <三氯矽烷的生成•回收> 於本實施形態的三氯矽烷製造裝置中，由四氯矽烷與 氫所成的原料氣體係通過位於反應爐1之底部的原料氣體 導入口 13而供應給反應容器10，於該處被加熱到約800 -19- 201034954 〜1300 °C左右而轉化成三氯矽烷與氯化氫。含三氯矽烷的 反應生成氣體係經由在反應容器10的反應生成氣體抽出 口 14所連接的抽出管2而導出到急冷塔4，與由急冷塔4 的上方所噴灑的冷卻液直接接觸•混合，而奪取冷卻液之 蒸發所伴隨的蒸發潛熱，瞬間地被冷卻600°C左右。然後 ，反應生成氣體係按照需要被再冷卻後，由急冷塔4的塔 頭取出而供到三氯矽烷的分離。 於本實施形態中，反應容器10由於以僅使其底部與外 〇 筒容器12接觸狀態被收納在外筒容器12內，藉由其自重 而固定在外筒容器12的底部，故不受到限制而可自由地 熱膨脹。又，抽出管2由於藉由在連結筒3內於抽出管2 與連結筒3之間與它們大致同軸地配之波紋管30所伸縮 自在地保持，故可自由地熱膨脹。 再者，藉由以波紋管30來伸縮自在地保持抽出管2的 一端，同時成爲反應容器10在其底部僅由自重來支撐的 構成，波紋管30不僅對於抽出管2，而且對於反應容器 ® 10的熱膨脹亦可追隨而變形。因此，波紋管30亦可吸收 在反應容器10及抽出管2所發生的任何應力，可保護裝 置全體防止變形或破損。 又，由於波紋管30遮斷反應爐1內部的空間與急冷塔 4內部的空間，故在遮斷構件沒有熱膨脹所致的變形或破 損，可更安定地維持兩塔間的氣密狀態。 再者，波紋管30係在連結筒3內部以覆蓋抽出管2的 方式所配置，高溫的外筒容器12內之空間與低溫的急冷 -20- 201034954 塔4內之空間係經由波紋管30進行熱交換’故可沿著波 紋管30在連結筒3內形成中間的溫度區域。因此，可分 散對抽出管2所施加熱負荷，可防止在抽出管2發生局部 的大應力。 又，於本實施形態中，如上述地’由於對於應力的發 生具有極優異的耐性，故即使與冷卻效率高的急冷系統倂 用，也不易損傷裝置。還有，由於抽出管2係從反應容器 10到急冷塔4爲止以直線最短距離連結，故可於平衡傾向 〇 於三氯矽烷側的狀態下將反應生成氣體送入急冷塔4，可 抑制三氯矽烷的消失。特別地，由於對所噴灑的冷卻液， 以反應生成氣體大略垂直地碰撞，可瞬間高效率地冷卻反 應生成氣體。 還有，由於進行三氯矽烷的轉化反應之反應容器10係 僅藉由反應容器10底部與外筒容器12相接，故可壓低反 應容器10與外筒容器12的接觸面積。因此，可抑制熱從 反應容器1 〇到外筒容器1 2的傳達，可抑制熱往外部逃， 〇 可提高從四氯矽烷到三氯矽烷的轉化效率。 尙且，本發明的技術範圍係不受上述實施形態所限定 ，在不脫離本發明的宗旨之範圍內，可加以各種的變更。 例如，爲了實現優異的耐久性或傳熱效率，反應容器 10本來較佳爲一體成形，但是由於製造技術上的問題，可 使用連結複數的大略圓筒體而一體化者。作爲大略圓筒體 以複數連結一體化的反應容器10，特別地較佳爲如第3圖 所示地’將複數的大略圓筒體51以端部彼此對接而大略 -21- 201034954 同軸地上下配置，由外側以環52來螺合締結 者。藉由成爲如此的構造，可使大略圓筒體5 爲單純者，由於形成壁厚爲薄的部位，故對於 具有優異的耐性。又，由於不是在連結部中一 筒體51之端部嵌合於另一方的大略圓筒體51 構成，故即使在高溫環境下使用而使大略圓筒 熱膨脹，也不會引起由於各個大略圓筒體51 數之不同所致的連結部之破裂或龜裂。因此， 0 反應容器10的構成構件之頻率，改善裝置的作 又，於上述實施態樣中，將波紋管30的反 部連接於連結筒3，將急冷塔4側端部連接於: 構成，但亦可與此相反地連接。即，波紋管30 內側的連接，係可藉由在急冷塔4的反應生成 口部42所設置的接合手段與在連結筒3所設 段之間夾入甜甜圈狀的板材31，在該板材31 3內的部分固定波紋管30的一端而進行，波怒 Ο 出管2外側的連接，係可藉由在構成抽出管2 21與第二構件22的連結部所形成的突出部25 3 0的一端而進行。 再者，於上述實施態樣中，抽出管2係由 構成，但是較佳爲由單一的構件所構成，因爲 理強度優異。又，取決於裝置的規模等，亦可 件所構成。 又，連接反應爐1與急冷塔4的連結筒3 對接的端部 1的構造成 物理的衝撃 方的大略圓 之端部般的 體5 1進行 的熱膨脹係 可減低交換 業效率。 應爐1側端 曲出管2而 與連結筒3 氣體導入開 置的接合手 伸出連結筒 :管30與抽 的第一構件 固定波紋管 3個構件所 耐熱性或物 由更多的構 較佳爲具備 -22- 201034954 具有波紋構造的波紋管。於此情況下，可藉由波紋管3 0 的形狀變化來吸收在連結筒3所發生的應力。因此，可防 止連結筒3之由於熱膨脹所致的破損，可提高裝置的安定 性、安全性。 實施例 以下藉由實施例來進一步說明本發明，惟本發明不受 此等所限定。 實施例1 〇 使用第1圖〜第3圖所示之三氯矽烷製造裝置來進行三 氯矽烷的製造，調查在反應容器及抽出管有無變形或破損。 <裝置說明> 於此裝置中使用以下的構件。 反應容器： 由外徑15cm、高度10cm、厚度3cm的等方向性石墨 所成的直圓筒狀之碳製大略圓筒體’準備複數個在自上端 起3.5cm的外周面及自下端起3.5cm的外周面設有陽螺紋 〇 部的碳製大略圓筒體。又’對於構成反應容器之頂蓋部的 上端側大略圓筒體及構成反應容器之底板部的下端側大略 圓筒體，亦同樣地在連結側的端部外周面設置陽螺紋部。 再者，於下端側大略圓筒體的底板之中央設置口徑 2.5cm、開口周圍的管狀突出部之高度10cm的原料氣體導 入口，於反應容器的軀體部上方所配置的一個大略圓筒體 之外周面設置口徑1.6cm的反應生成氣體抽出口。 其次，爲了在此等的碳製大略圓筒體之內周面及外周 -23- 201034954 面形成碳化矽被膜，於CVD反應裝置內設置碳製大略圓筒 體，以氬氣置換裝置內部，加熱到1200 °C。於CVD反應 裝置內導入三氯甲基矽烷與氫的混合氣體（莫耳比1:5)，藉 由CVD法，在碳製大略圓筒體的全表面上形成200μιη的 厚度之碳化矽被膜。 接著，準備複數個由內徑15cm、上下方向的寬度 7.5cm、徑向的厚度3.6cm的等方向性石墨所成的碳製環， 其爲在內周面形成有與前述碳製大略圓筒體所形成的陽螺 〇 紋部螺合之陰螺紋部的碳製環，與上述同樣地在其全表面 上施予碳化矽被膜。 使用此等的碳製大略圓筒體及碳製環來構成反應容器 〇 抽出管： 使用由直線狀連結在連結端部具有凸緣的3支中空管 所構成的碳製抽出管。對於碳製抽出管，亦與上述同樣地 在全表面上施予碳化矽被膜。 〇 所組裝的抽出管係全長40cm、外徑3cm。 波紋管： 使用全長11cm、入口徑4cm、軸向的位移量爲5%、與 軸垂直方向的位移量爲4%的不銹鋼鋼製之波紋管。 <裝置的組裝> 於內部具備加熱器的底部及於外周面分別具備原料氣 體導入開口部和反應氣體抽出開口部的外筒容器中，以使 反應容器的原料氣體導入口之管狀突出部嵌合於外筒容器 -24- 201034954 的原料氣體導入開口部，同時以使反應容器的反應生成氣 體抽出口與外筒容器的反應氣體抽出開口部成一致的方式 ’收納反應容器。接著，將抽出管的一端由外筒容器的反 應氣體抽出開口部插入而連接於反應容器的反應生成氣體 抽出口，將波紋管的一端接合於抽出管的外周，將另一端 接合於連結筒的內周，將連結筒的一端連接於外筒容器的 反應氣體抽出開口部，將另一端連接於急冷塔的反應生成 氣體導入開口部。 Ο 〈實驗條件〉 使用上述裝置，於反應爐中在常壓、1100 °c的反應溫 度下使四氯矽烷與氫（莫耳=1:1)的原料氣體反應，經由抽 出管取出反應生成氣體而送到急冷塔，噴吹經溫度調節在 2(TC的冷卻液（三氯矽烷濃度20%)來冷卻。由急冷塔所導 出的冷卻後之反應生成氣體的溫度爲30°C。 <實驗結果> 連續地運轉此三氯矽烷製造裝置2000小時後，將裝置 〇 解體，觀察反應容器、抽出管及連結筒，結果在任一構件 , 皆沒有觀察到變形或破損。 比較例1 除了代替波紋管，配設沒有波紋構造的筒狀構件（厚度 :2mm)以外，與上述實施例1同樣地調整三氯矽烷製造裝 置。此筒狀構件係由與實施例1使用的波紋管相同的材質 所構成，與連結筒或抽出管的接合方法亦與實施例1同樣 -25- 201034954 與實施例1同樣地運轉此三氯矽烷製造裝置，將裝置 解體，觀察反應容器、抽出管、連結筒及筒狀構件，結果 在抽出管與筒狀構件看到變形。 比較例2 除了代替波紋管，使用具有抽出管可貫穿的開口之平 面板狀構件（厚度：2mm)，在連結筒的中央附近遮斷反應 爐側的空間與急冷塔側的空間以外，與上述實施例1同樣 地調整三氯矽烷製造裝置。此平面板狀構件係由與實施例 Ο 1使用的波紋管相同的材質所構成。 與實施例1同樣地運轉此三氯矽烷製造裝置，將裝置 解體，觀察反應容器、抽出管、連結筒及平面板狀構件， 結果在與板狀構件的接合部位中於抽出管看到變形。 比較例3 除了以反應容器的頂蓋部接觸外筒容器的天花板 (ceiling)而固定之方式，配設厚的外筒容器天花板部之絕 熱材以外，與上述實施例1同樣地調整三氯矽烷製造裝置 〇 與實施例1同樣地運轉此三氯矽烷製造裝置’結果外 筒容器天花板部的外表面之溫度與實施例1的情況相比亦 上升30%，確認反應容器的熱洩漏到外部。又’在反應容 器看到龜裂，於到達2000小時之前變成不可能連轉。 <實驗的考察> 如由以上的比較實驗可明知，藉由以波紋管來伸縮自 在地保持抽出管的一端，同時成爲反應容器係在其底部僅 -26- 201034954 由自重來支撐的構成，可保護裝置全體防止變形或破損。 又，由於反應容器與外筒容器的接觸面積變少，故可抑制 熱從反應容器到外部的洩漏，可謀求三氯矽烷的生產效率 之提高。 以上係以實施例爲基礎來說明本發明。此實施例終究 是例示而已，本業者理解各種的變形例係可能，而且該變 形例亦在本發明的範圍內。 【圖式簡單說明】 0 第1圖係本發明的實施形態之三氯矽烷製造裝置的說 明圖。 第2圖係本發明的實施形態之三氯矽烷製造裝置的連 結筒周邊之示意縱剖面圖》 第3圖係顯示本發明所可使用的反應容器之一實施態 樣的示意縱剖面圖。 【主要元件符號說明】 I 反應爐 〇 2 抽出管 3 連結筒 4 急冷塔 10 反應容器 II 加熱器 12 外筒容器 原料氣體導入口 反應生成氣體抽出口 -27- 14 201034954 15 16 18 19 2 1 22 23 Ο 24 25 30 3 1 40 4 1 42 ❹ 發熱體 電極 原料氣體導入開口部 反應生成氣體抽出開口部 管狀突出部 第一構件 第二構件 第三構件 反應生成氣體噴出部 突出部 波紋管 板材 金屬製容器 反應生成氣體導入開口部 大略圓筒體 環 -28-SiCl4 + H2 〇 SiHCl3 + HC1 (1) This reaction is carried out by heating a raw material gas composed of vaporized tetrachloromethane and hydrogen to 800 ° C to 1300 ° C in a reaction vessel.高温 In the high-temperature reaction product gas discharged from the reaction vessel, in addition to the trichloromethane and hydrogen chloride formed, a large amount of unreacted tetrachloroporphyrin and hydrogen are contained. In order to take out trichloromethane from the reaction product gas, a method of condensing in a distillation column using a difference in boiling points of tetrachlorosilane and trichloromethane is used. Specifically, 'in the condenser' is divided into a condensed portion of chlorodecane and an uncondensed portion of hydrogen chloride, hydrogen, and an uncondensed chloramphenicol, and then cooled to about -70 ° C by cryogenic separation to obtain a condensed portion. Trichlorodecane was isolated. When the desired trichloromethane is separated from the reaction product gas, if the reaction gas generated at a high temperature immediately after the -4-201034954 is discharged from the reaction vessel is suddenly introduced into the distillation column, an excessive load is applied to the distillation column. Therefore, it is necessary to preliminarily cool in the quenching tower before introducing the reaction product gas into the distillation column. However, even if so-called preliminary cooling, if the cooling power is not very large, the equilibrium tends to be on the tetrachloromethane side, and the resulting trichloromethane is returned to tetrachloromethane again. Therefore, in order to improve the recovery efficiency of the trichloromethane, it is necessary to freeze the 〇 reaction product gas to a predetermined temperature as soon as possible, and to freeze the equilibrium at the time when the equilibrium is sufficiently reached on the trichloromethane side. In order to freeze the above equilibrium state instantaneously, it is necessary to rapidly cool the reaction product gas to about 600 C within 1 second. A reaction vessel having a mechanism for converting tetrachlorosilane with hydrogen to convert it to trichloromethane and cooling the reaction product gas is disclosed, for example, in Patent Document 1. According to the reactor described in this document, a heat exchanger is connected to the bottom of the reactor, and a raw material gas of hydrogen and chlorosilane which is preheated in the heat exchanger is supplied to the reactor. The supplied raw material gas system is advanced upward in the outer chamber provided in the reactor, and is heated by the heating element provided in the reactor. The gas system generated by heating changes the direction of progress by the diverter disposed at the upper portion of the reactor, advances to the bottom portion in the inner chamber of the reactor, and then flows into the heat exchanger, which is generated by the heated reaction in the heat exchanger. The gas is thermally transferred to the raw material gas supplied to the reactor. Thereby, the reaction product gas is cooled, and the material gas is preheated. Further, as another example, there is a description in Patent Document 2. In this document, a device for producing chloroformane is proposed, which comprises a reaction vessel for supplying a supply gas containing tetrachloromethane and hydrogen to the inside to form a reaction product gas containing trichlorosilane and hydrogen chloride, and heating the inside of the reaction vessel. The heating mechanism 'the storage container accommodating the reaction container and the heating mechanism' supplies the gas supplied to the reaction container to the inner cylinder, and the gas disposed substantially coaxially outside the gas supply inner cylinder is supplied to the outer peripheral surface of the inner cylinder and the inner peripheral surface of the inner cylinder. A gas exhaust outer cylinder 'which forms an exhaust gas flow path for generating a reaction gas, and a cooling cylinder that supports a gas exhaust outer cylinder on the inner side and has a refrigerant passage through which the refrigerant flows. In the chloroformane manufacturing apparatus, the reaction product in the high temperature state generates a gas enthalpy when it flows through the exhaust gas flow path, and the refrigerant flows through the cooling cylinder provided outside the gas exhaust outer cylinder to be externally At the same time as cooling, the gas supplied to the inside of the gas exhaust outer cylinder is supplied to the inside of the reaction vessel, and is exchanged with the inflowing supply gas to be cooled. That is, the cooling efficiency is improved by simultaneously cooling from the inside and the outside of the gas exhaust outer cylinder. However, in the reactor described in Patent Document 1, the cooling of the reaction product gas is only required to cool the reaction product gas of up to 1000 ° C or more to 600 in the case of heat exchange with the raw material gas that is adjoining. It is difficult to get around °c. Therefore, the balance is gradually inclined to the tetrachloromethane side until the reaction product gas is discharged, and a part of the trichloromethane which is not easily formed is lost. Further, in the device described in Patent Document 2, a cooling cylinder in which a refrigerant passage is formed around the gas exhaust outer cylinder is provided. However, in this case, the cooling of the reaction product gas is via the gas exhaust outer cylinder. The inner wall and the outer wall are heat exchanged, so it may not be sufficient to say that the cooling rate and capacity are sufficient. -6- 201034954 Further, in the apparatus described in Patent Document 2, the bottom of the reaction container is closed by the lower support circular plate, and since the lower support circular plate is only formed at the central portion thereof by the bottom plate constituting the storage container The support member of the bottom support member protrudes upward from the center, so that even if the wall of the reaction tube constituting the reaction vessel is thermally expanded, the lower support circular plate system can support the column member as a center and flexure and deform, and can absorb the stress. However, although the gas exhausting outer cylinder or the gas exhaust pipe through which the high-temperature reaction generating gas passes is disposed in the upper portion of the reaction vessel, the upper portion of the reaction vessel is supplied to the inner cylinder and the upper ring by the upper support circular plate and the gas. The plate and the gas are exhausted from the outer tube and are in contact with the storage container, and are supported and fixed. In other words, the gas discharge outer cylinder and the gas exhaust pipe through which the high-temperature gas flows are supported and fixed by the storage container, the top plate portion, the cooling cylinder, and the supply gas introduction portion, so that stress concentration due to thermal expansion of the member cannot be alleviated. It is easy to cause deformation or breakage. Further, since the low-temperature cooling cylinders are disposed adjacent to each other outside the gas exhaust outer cylinder, if the cooling capacity is excessively increased, a local excessive temperature difference occurs in each of the members constituting the portion, and stress is concentrated to cause breakage. After that. Therefore, as a method of cooling the reaction product gas more strongly and instantaneously, for example, by the cooling method of the inner wall or the outer wall of the exhaust pipe, it is proposed to export the reaction product gas from the high-temperature reaction vessel to the quenching tower, and to make it The method in which the coolant directly contacts the reaction product gas and extracts heat from the reaction product gas by the latent heat of vaporization when the coolant is vaporized. For example, Patent Document 3 proposes an apparatus comprising: introducing a tetrachlorosilane and hydrogen into a reaction chamber to obtain a reaction gas containing a mixture of trichlorosilane and hydrogen chloride at a temperature of 60 (TC to 120 (TC). After -7-201034954, a gas is generated by the reaction derived from the reaction chamber, and a mixture of the chlorodecane mixture cooled to room temperature is sprayed to be cooled, and the cooling means is cooled to 3 ° C or less within 1 second. [Patent Document 1] JP-A-2008- 1 3 3 1 7 5 (Patent Document 3) Japanese Patent Publication No. Sho 57-3 8524 [Summary of the Invention] In the apparatus described in Patent Document 3, the reaction furnace and the quenching tower are connected via a connecting pipe provided on the side of the quenching tower, and a closed end portion is formed at the joint portion between the connecting pipe and the reaction furnace. The closed end, through which the reaction gas generated by the reaction furnace is led to the quenching chamber. However, the high temperature reactor and the low temperature quenching chamber are closed by the joint between the connected tube and the reaction furnace. Wall Because of the shielding, a large local temperature difference occurs between the quenching tower and the end wall surface of the reactor and the vicinity of the reactor. As a result, the stress caused by the thermal expansion is concentrated on the portion, and the crucible is deformed or damaged. The fixed probe is also thermally expanded, and the stress is concentrated on the joint between the probe and the end wall surface, and is deformed or broken. That is, the system is excellent in rapid cooling in a system in which a cooling liquid is directly sprayed to the reaction product gas and is instantaneously cooled. On the other hand, since there is a local large temperature difference in the device, how to avoid stress concentration due to thermal expansion becomes a problem. However, Patent Document 3 does not touch at all the means for absorbing or relieving the stress. The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a device for producing triclosan which is less likely to undergo deformation or breakage due to thermal expansion, and has excellent recovery efficiency of trichloromethane and excellent conversion efficiency of trichlorodecane. In order to solve the above problems, the following configuration is adopted. That is, the trichloromethane manufacturing apparatus of the present invention The present invention is characterized in that it has a substantially cylindrical reaction vessel for producing a reaction gas containing trichlorosilane and hydrogen chloride from a raw material gas containing tetrachlorosilane and hydrogen, a heater for describing the reaction vessel before heating, and a reaction for storing the reaction. a reactor and a heater, and a reaction furnace for the outer cylinder container in which the reaction vessel is only in contact with the bottom of the reaction vessel, the quenching tower in which the reaction gas is cooled, and the connecting cylinder connected between the reactor and the quenching tower are passed through a drawing tube for discharging the reaction product gas to the quenching tower in a reaction furnace, which is disposed so as to reach the quenching tower inside the connecting cylinder, which is substantially perpendicularly connected to the outer peripheral surface of the reaction vessel, and is connected to the connecting tube The inside is arranged substantially coaxially so as to cover the above-mentioned extraction pipe, and one end is joined to the inner circumference of the connection cylinder, and the other end is joined to the bellows of the outer circumference of the extraction pipe. <Prevention of damage due to thermal expansion> In the apparatus for producing trichloromethane of the present invention, the reaction container is stably housed in the reaction furnace in a state where only the bottom portion thereof is in contact with the bottom of the outer cylinder container. Here, the reaction vessel is connected to one end of the extraction pipe on the outer peripheral surface thereof, and since the extraction pipe is held in the interior of the coupling cylinder by a retractable bellows to maintain 201034954, it does not substantially contribute to the fixation of the reaction vessel, nor does it The reaction vessel exerts an excessive pushing force. That is, the reaction container is housed in the outer cylinder container only in a state where the bottom portion thereof is in contact with the outer cylinder container, and is fixed to the bottom of the outer cylinder container by its own weight, without any fixing means, even if heating occurs. The thermal expansion does not cause stress concentration, and the extraction pipe is kept stretched and contracted by the bellows disposed substantially coaxially between the extraction pipe and the connection cylinder in the connection cylinder, so even if the crucible is reacted The generated gas is heated and thermally expanded by passage, and can be expanded and contracted by the bellows to avoid concentration of stress. However, by retaining one end of the extraction tube freely by the bellows, and at the same time, the reaction container is supported by the bottom portion only by its own weight, the bellows can not only thermally expand the extraction tube but also thermally expand the reaction container. Follow and deform. Therefore, even if the thermal expansion of both the reaction container and the extraction tube is performed, the deformation can be appropriately absorbed to absorb the stress, and the entire device can be protected from deformation or breakage. 〇 In addition, the bellows also serves as a blocking member for interrupting the space inside the reactor and the space inside the quenching tower. Since it can be freely deformed, the airtight state between the two towers can be maintained more stably. Further, in the apparatus for producing chloroformane, in order to generate a gas generated by the reaction in the reaction vessel in the reactor, the gas is led to the quenching tower through the extraction pipe which is vertically connected to the outer peripheral surface of the reaction vessel. It is connected by the shortest distance of the straight line from the reaction vessel to the quench tower. Therefore, the extraction pipe can be a substantially linear hollow pipe, and since it does not need to be a complicated -10-201034954 shape, it is excellent in heat resistance. That is, in the case where the extraction pipe is held by the bellows, when the extraction pipe is bent, it is likely to have a large stress on the bent portion of the extraction pipe or the continuous portion of the reaction vessel due to the strength of expansion and contraction of the bellows or the like. However, in this trichloromethane manufacturing apparatus, since the extraction pipe is simply a straight line, the extraction pipe does not load a local excessive stress. Further, since the bellows is disposed inside the connecting cylinder so as to cover the extracting pipe, an intermediate temperature region of the two spaces can be formed in the region. That is, in the connection cylinder, an intermediate temperature region which gradually descends from the outer cylinder container side to the quenching tower side is formed, and the heat load applied to the extraction pipe can be dispersed. Therefore, it is possible to prevent local large stress from occurring in the extraction pipe. In this way, the end of the extraction tube is freely stretched by the bellows, and the reaction container is supported by the self-weight at the bottom thereof, and the reaction container and the extraction tube exposed to the high temperature are freely expanded or contracted. It can avoid the concentration of stress and protect the whole device from deformation or damage. <Improvement of recovery efficiency> As described above, the apparatus for producing triclosan of the present invention has excellent resistance to the occurrence of stress, and therefore can be used in a quenching system having high cooling efficiency. Therefore, for example, in the inside of the quenching tower, it is particularly suitable to directly spray the cooling liquid into the reaction-generating gas taken in, and to use the latent heat of vaporization at the time of vaporization of the cooling liquid to instantaneously take the heat type. In this case, the latent heat of vaporization accompanying the vaporization of the cooling liquid is much higher than the case where the heat is exchanged with the refrigerant or the supply gas by the wall of the exhaust gas flow path forming the reaction product gas. Cooling is carried out efficiently and economically. -11- 201034954 Further, by arranging the extraction tube to the quenching tower linearly and vertically with respect to the outer peripheral surface of the reaction vessel, the distance from the reaction vessel to the quenching tower can be minimized. Therefore, it can be supplied to the quenching tower in a short period of time in a state of being balanced toward the trichloromethane side, and the amount of trichloromethane which the reaction product gas is cooled by flowing between the extraction tubes can be reduced. Further, by adopting such a configuration, since the extraction pipe system is inserted into the quenching tower substantially horizontally, the reaction product gas is also ejected substantially horizontally. In general, in the method of spraying the cooling liquid to the reaction product gas, the cooling liquid is sprayed from the upper side to the lower side of the quenching tower, and the cooling liquid accumulated in the lower portion of the quenching tower due to gravity is sent to the cooling device for cooling, and then used. The circulation system that is pumped to the upper part of the cooling tower for re-spraying. In the chloroformane manufacturing apparatus, when the cooling liquid is sprayed from the upper side to the lower side of the cooling tower, the reaction product gas can be ejected substantially horizontally, so that the reaction product gas can collide with the cooling liquid substantially vertically. As a result, both can be surely mixed, and cooling can be performed efficiently. Moreover, since the spray direction of the cold liquid is substantially vertical with respect to the axial direction of the extraction pipe, the sprayed coolant liquid flows into the inside of the extraction pipe to be low, and the extraction pipe or the reaction container can also be protected. The interior prevents corrosion. As a result, the recovery efficiency of the trichloromethane can be greatly improved by rapidly and efficiently cooling the reaction-forming gas in a state in which the balance tends to be trichloromethane. <Improvement of Conversion Efficiency> Further, since the -12-201034954 reaction of tetrachlorosilane and hydrogen to form trichloromethane in the above formula (1) is an endothermic reaction, in order to increase the conversion efficiency of trichloromethane, at least the reaction must be made. The heat inside the container does not escape. In the apparatus for producing triclosan of the present invention, since the reaction vessel for carrying out the conversion reaction of trichloromethane is in contact with the outer cylinder container only at the bottom of the reaction vessel, the contact area between the reaction vessel and the outer cylinder vessel can be lowered. As a result, the transfer of heat from the reaction vessel to the outer cylinder container can be suppressed, and heat can be suppressed from being escaped to the outside. Therefore, conversion efficiency from tetrachlorodecane to trichlorodecane can be provided. As described above, according to the apparatus for producing triclosan of the present invention, the end portion of the extraction tube is freely stretched by the bellows, and the reaction container is supported by the self-weight at the bottom thereof, and the reaction container and the extraction are carried out. The pipe system is free to expand or contract to avoid stress concentration, and the entire device can be protected from deformation or breakage. Therefore, as the heat resistance is improved, it is possible to use a quenching system having a high cooling efficiency, and it is possible to recover trichloromethane more efficiently than before without damaging the equipment. Further, by the above configuration, since leakage of heat from the reaction container to the outside can be suppressed, the conversion efficiency of trichloromethane can be improved.如此 In this way, the productivity of trichlorodecane can be improved by simultaneously improving the above-mentioned heat stability, recovery efficiency, and conversion efficiency. [Embodiment] Hereinafter, embodiments of the present invention will be described using the drawings. Moreover, in all the drawings, the same components are denoted by the same reference numerals, and the description is appropriately omitted. Fig. 1 is a view schematically showing an embodiment of the apparatus for producing triclosan according to the present invention. Further, Fig. 2 is a view schematically showing a cross section of the periphery of the connecting cylinder of the trichloromethane producing apparatus -13 - 201034954. As shown in Fig. 1 and Fig. 2, the apparatus for producing triclosan of the present embodiment includes a rough circle containing a reaction gas containing trichlorosilane and hydrogen chloride from a raw material gas containing tetrachlorosilane and hydrogen. a cylindrical reaction vessel 10, a heater 11 for heating the reaction vessel 10, and a reaction furnace 1 for housing the outer cylinder vessel 12 in which the reaction vessel 10 and the heater 11 are housed and the reaction vessel 10 is only in contact with the bottom of the reaction vessel 10. The quenching tower 4 in which the gas is cooled by the reaction, and the connecting cylinder 3 connected between the reactor 1 and the quenching tower 4 is connected to the inside of the connecting cylinder 3 which is vertically and vertically connected to the outer peripheral surface of the reaction vessel 10 The extraction tube 2 that leads the reaction product gas to the quenching tower 4 in the reaction furnace 1 disposed in the manner of reaching the quenching tower 4, and is disposed substantially coaxially inside the connecting tube 3 so as to cover the extraction tube 2, One end is joined to the inner circumference of the coupling cylinder 3, and the other end is joined to the bellows 30 of the outer circumference of the extraction tube 2. <Reaction Furnace> The reaction furnace 1 includes a reaction vessel 10, a long heater 11 disposed to surround the outer side of the reaction vessel 10, and an outer cylinder vessel 12 accommodating the reaction vessel 10 and the heater 11. The reaction vessel 10 is maintained at a high temperature of about 800 ° C to about 1 300 ° C by heating the outer wall of the reaction vessel 1 以 by the heater 11 inside the insulated outer cylinder vessel 12 The mixed gas of tetrachloro-14-201034954 decane and hydrogen supplied from the raw material gas inlet 13 provided at the bottom is reacted inside the reaction vessel 10 to form a reaction product gas containing trichlorosilane and hydrogen chloride. <Reaction vessel> The reaction vessel 10 is a substantially cylindrical container for reacting tetrachlorosilane with hydrogen in a high-temperature environment, and has a raw material gas introduction port 13 for taking in a material gas, and is connected to a later-described extraction. The reaction of the tube 2 for deriving the reaction-forming gas generates a gas extraction port 14. In the present embodiment, the raw material gas introduction port 13 is provided at the center of the bottom of the reaction container 10, and the reaction product 〇 gas extraction port 14 is provided on the outer peripheral surface of the reaction container 10. The material gas introduction port 13 is formed so as to be formed in a tubular protruding portion 19 from the bottom portion of the outer casing 12 to be described later. It is preferred that the inner peripheral surface and/or the outer peripheral surface of the reaction vessel 10 be treated with a tantalum carbide coating. Since the tantalum carbide film is extremely resistant to chemical decomposition, chemical etching of the carbon structure can be prevented. Therefore, the surface of the reaction vessel 10 can be protected from corrosion by the treatment of the niobium carbide film.加热器 <Heater> The heater 11 includes a plurality of long strip-shaped carbon heat generating bodies 15 extending in the vertical direction, and an electrode 16 for supplying electric power to the heat generating body 15 connected to one end of the heat generating body 15. The heater 11 is disposed so as to surround the periphery of the reaction vessel 10, and the temperature inside the reaction vessel 10 is adjusted from the outside of the reaction vessel 1 by controlling the amount of supplied electric power. <Outer-tube container> The outer-tube container 1 2 is a substantially cylindrical container in which the outer side is made of a metal such as stainless steel, and the inner side is covered with a heat insulating material such as a -15-201034954 carbon plate, a refractory brick, or a heat insulating brick. The outer cylinder container 12 houses the reaction container 10 and the heater 11 to insulate them from the outside. In the outer cylinder container 12, the raw material gas introduction opening portion 17 and the reaction product gas extraction opening portion 18 are provided at positions corresponding to the material gas introduction port 13 and the reaction product gas extraction port 14 when the reaction container 10 is housed. The reaction product gas extraction opening portion 18 is provided with a joining means such as a flange, and may be connected to a connecting cylinder 3 to be described later.原料 The material gas introduction opening portion 17 is fitted to the bottom of the reaction container 10, and the tubular projecting portion 19 as the material gas introduction port 13 is fitted, and the diameter thereof is substantially the same as the outer diameter of the tubular projecting portion 19. When the reaction container 10 is housed in the outer cylinder container 12, the raw material gas provided in the bottom of the outer cylinder container 12 is introduced into the opening portion 17, and the tubular projecting portion 19 provided at the bottom of the reaction container 10 is fitted to secure the reaction container. The inflow path of the material gas is positioned to be fixed while being fixed to the bottom of the outer cylinder container 12 by the own weight of the reaction vessel 10. 〈 <Connection Tube> The connection tube 3 has a joining means connected to the reaction furnace 1 at one end, and has a joining means connected to the quenching tower 4 at the other end. The connecting cylinder 3 of the present embodiment is made of a metal such as stainless steel, and as shown in Fig. 2, the flange 'having a reaction-generating gas extraction opening 18 that is connectable to the outer cylinder container 12 at one end has the other end. A flange for connecting the reaction product gas introduction opening portion 42 to the quenching tower 4 to be described later. <Quench Tower> -16· 201034954 The quenching tower 4 includes a cylindrical metal container 40, a nozzle 41 for spraying a coolant in the container provided in the container, and a coolant stored in the bottom of the container. a pump that is circulated to the nozzle 41 (mainly shown), a cooling device for cooling the cooling liquid (illustrated in abbreviated form), and a conduit for taking out the cooled reaction-generated gas from the top of the quenching tower 4 (provincial sketch) Show). A reaction gas introduction opening portion 42 for connecting the connection tube 3 is provided on the side wall of the quenching tower 4, and a bonding means such as a flange for connecting to the connection tube 3 is provided in the reaction product gas introduction opening portion 42. The nozzle 41 is provided in the vicinity of the upper portion of the reaction product gas introduction opening portion 42 so as to generate a gas into the reaction introduced into the quenching tower 4 and spray the coolant from the upper side. The cooling liquid for cooling the reaction product gas is composed, for example, of a mixture of trichloromethane and tetrachlorosilane, and the ratio of tetrachloromethane to the total amount of tetrachlorosilane and trichloromethane is 1 ~0.5. The temperature is preferably 60 ° C or less. For example, it is preferred to use a composition ratio of tetrachlorosilane:trichlorosilane of 85:15 and a temperature of about 40 °C.冷却 The cooled reaction product gas system taken out from the top of the quenching tower 4 is sent to the distillation column via a conduit to separate the desired trichlorosilane. <Extraction pipe> The extraction pipe 2 connects the inside of the reaction vessel 10 and the carbon tubular member inside the quenching tower 4 through the inside of the connection cylinder 3, and the reaction product gas in the reaction vessel 10 is led to the quenching tower 4. The material constituting the extraction tube 2 is a graphite material having excellent airtightness, and in particular, from the viewpoint of high strength and thermal expansion due to the fine particle structure, it is preferable to use heat resistance and corrosion resistance in any direction from -17 to 201034954. Also excellent in isotropic high purity graphite. In particular, it is preferable that the inner circumferential surface and/or the outer circumferential surface of the extraction tube 2 is treated with a ruthenium carbide film formed by a CVD method at a thickness of 10 to 500 μm. Since the tantalum carbide film is extremely resistant to chemical decomposition, chemical leaching of uranium into the carbon structure can be prevented. Therefore, the surface of the extraction tube 2 can be protected from corrosion by the treatment of the ruthenium carbide film. The extraction pipe 2 of the present embodiment is composed of a plurality of members, and when the crucible device is assembled, the first member 21 mainly located in the reaction furnace 1, the second member 22 mainly located in the connection cylinder 3, and the main The third member 23 is located in the cooling tower. That is, the first member 21 has a connection portion with the reaction product gas extraction port 14 of the reaction container 10 at one end, and a joining means for coupling the second member 22 at the other end, and the second member 22 is provided at both ends. In the joining means for joining the first member 21 or the third member 23, the third member 23 has a joining means for joining the second member 22 at one end, and a reaction product generating gas discharge portion 24 at the other end.接合 The joining means of the drawing pipe 2 is such that the protruding portion 25 is formed on the outer peripheral side of the drawing pipe 2 so as to join the bellows 30 to be described later. As the joining means for forming such a projection 25, a flange can be typically used. Further, a substantially cylindrical tubular member may be used, and the abutting end portion may be screwed and joined by a ring from the outside. In this case, the ring system forms a projection 25 for fixing the bellows 30. <Corrugated pipe> The bellows 30 is a member of a corrugated structure made of metal, which is expandable and contractible in the direction of the axis -18-201034954, and is also deformable in the radial direction. The bellows 30 may be made of metal, more preferably stainless steel, and may be made of Worthite iron stainless steel or fat iron stainless steel. The bellows 30 is preferably 2 to 10% of the height of the mountain entrance, and the distance between the mountain and the mountain is about 2 to 8%. Further, it is preferable that the amount of displacement in the axial direction is 3 to 10% of the diameter of the inlet, and the amount of displacement in the direction perpendicular to the axis is about 2 to 5% of the total length. Also, the spacing or height of the mountains may be uniform or non-uniform. The bellows 30 is disposed substantially coaxially inside the connecting cylinder 3 so as to cover the outer side of the drawing pipe 2, and one end is joined to the inner circumference of the connecting cylinder 3, and the other end is joined to the outer circumference of the drawing pipe 2. In the present embodiment, the connection between the bellows 30 and the inner circumference of the connecting cylinder 3 is made by the joining means provided in the reaction-generating gas extraction opening 18 of the outer cylinder container 12 and the joining means provided in the connecting cylinder 3. The donut-shaped plate member 31 is sandwiched, and a portion of the plate member 31 that protrudes from the connecting tube 3 is fixed to one end of the bellows 30. Further, the connection between the bellows 30 and the outer circumference of the extraction pipe 2 is performed by fixing one end of the bellows 30 to the flange used for the connection between the second member 22 and the third member 23 constituting the extraction pipe 2. The bellows 30 securely retains the extraction pipe 2 while hermetically blocking the high temperature space inside the reaction furnace 1 and the low temperature space inside the quenching tower 4. <Production and Recovery of Trichlorodecane> In the apparatus for producing chloroformane of the present embodiment, a raw material gas system composed of tetrachlorosilane and hydrogen is supplied through a raw material gas introduction port 13 located at the bottom of the reaction furnace 1. The reaction vessel 10 is heated to a temperature of about 800 -19 to 201034954 to 1300 ° C where it is converted to trichloromethane and hydrogen chloride. The trichloromethane-containing reaction-generating gas system is led to the quenching tower 4 via the extraction pipe 2 connected to the reaction-generating gas extraction port 14 of the reaction vessel 10, and is directly contacted and mixed with the coolant sprayed from above the quenching tower 4. The latent heat of vaporization accompanying the evaporation of the cooling liquid is captured, and is instantaneously cooled to about 600 °C. Then, the reaction product gas system was recooled as needed, and then taken out from the column of the quenching tower 4 to supply the separation of trichloromethane. In the present embodiment, the reaction container 10 is housed in the outer tube container 12 in a state in which only the bottom portion thereof is in contact with the outer tube container 12, and is fixed to the bottom portion of the outer tube container 12 by its own weight, so that it is not limited. Free thermal expansion. Further, since the extraction pipe 2 is held by the bellows 30 which is substantially coaxially disposed between the extraction pipe 2 and the connection cylinder 3 in the connection cylinder 3, it can be freely thermally expanded. Further, by one end of the extraction tube 2 by the bellows 30, the reaction container 10 is supported by its own weight at its bottom, and the bellows 30 is not only for the extraction tube 2 but also for the reaction container®. The thermal expansion of 10 can also follow and deform. Therefore, the bellows 30 can also absorb any stress generated in the reaction container 10 and the extraction tube 2, and can protect the entire device from deformation or breakage. Further, since the bellows 30 blocks the space inside the reaction furnace 1 and the space inside the quenching tower 4, the blocking member does not undergo deformation or breakage due to thermal expansion, and the airtight state between the two towers can be maintained more stably. Further, the bellows 30 is disposed inside the connecting cylinder 3 so as to cover the extraction pipe 2, and the space in the high-temperature outer cylinder container 12 and the low-temperature quenching -20- 201034954 in the tower 4 are via the bellows 30. The heat exchange 'causes the intermediate temperature zone in the connecting cylinder 3 along the bellows 30. Therefore, the heat load applied to the extraction pipe 2 can be dispersed, and local large stress can be prevented from occurring in the extraction pipe 2. Further, in the present embodiment, as described above, since the stress is extremely excellent, even if it is used in a quenching system having a high cooling efficiency, the device is less likely to be damaged. Further, since the extraction pipe 2 is connected at the shortest distance from the reaction vessel 10 to the quenching tower 4, the reaction product gas can be sent to the quenching tower 4 in a state where the equilibrium tends to be on the trichloromethane side, and the three can be suppressed. The disappearance of chlorodecane. In particular, since the reaction liquid is substantially vertically collided with respect to the sprayed coolant, the reaction product gas can be efficiently cooled in an instant. Further, since the reaction vessel 10 for carrying out the conversion reaction of trichlorodecane is brought into contact with the outer cylinder container 12 only by the bottom of the reaction vessel 10, the contact area between the reaction vessel 10 and the outer cylinder vessel 12 can be lowered. Therefore, the transfer of heat from the reaction vessel 1 to the outer cylinder container 12 can be suppressed, the heat can be prevented from being escaped to the outside, and the conversion efficiency from tetrachloromethane to trichloromethane can be improved. The technical scope of the present invention is not limited to the above-described embodiments, and various modifications can be made without departing from the spirit and scope of the invention. For example, in order to achieve excellent durability or heat transfer efficiency, the reaction container 10 is preferably integrally formed. However, due to manufacturing problems, it is possible to integrate a plurality of substantially cylindrical bodies. As the reaction vessel 10 in which the substantially cylindrical body is integrated in a plurality of joints, it is particularly preferable to "connect the plural large cylindrical bodies 51 at the ends with the ends as shown in Fig. 3, roughly - 21 - 201034954. The arrangement is made by a ring 52 from the outside to screw the contractor. With such a structure, the roughly cylindrical body 5 can be made simple, and since it has a thin wall portion, it has excellent resistance. Further, since the end portion of the cylindrical body 51 is not fitted to the other substantially cylindrical body 51 in the joint portion, even if it is used in a high-temperature environment, the large cylinder is thermally expanded, and it does not cause a slight circle. Cracks or cracks in the joint due to the difference in the number of cylinders 51. Therefore, the frequency of the constituent members of the reaction vessel 10 is improved, and in the above embodiment, the reverse portion of the bellows 30 is connected to the connecting cylinder 3, and the end portion of the quenching tower 4 is connected to: But it can also be connected in reverse. That is, the connection inside the bellows 30 can be formed by sandwiching a donut-shaped plate 31 between the joining means provided in the reaction generating opening portion 42 of the quenching tower 4 and the section provided in the connecting cylinder 3. The portion of the plate member 31 3 is fixed to one end of the bellows 30, and the connection of the outside of the tube 2 is made by the protrusion 25 3 formed at the joint portion of the extraction tube 21 and the second member 22. One end of 0 is performed. Further, in the above embodiment, the extraction tube 2 is constituted, but it is preferably composed of a single member because it is excellent in physical strength. Further, depending on the size of the device, etc., it may be constructed. Further, the thermal expansion of the body 5 1 which is connected to the end portion 1 of the reaction furnace 1 and the connection tube 3 of the quenching tower 4, which is configured to be physically rounded, can reduce the efficiency of the exchange. The joint hand 2 of the furnace 1 is bent out and the gas is introduced into the connecting cylinder 3 to extend the connecting cylinder: the tube 30 and the drawn first member fix the bellows. The heat resistance of the three members is more It is preferable to have a bellows having a corrugated structure of -22-201034954. In this case, the stress generated in the connecting cylinder 3 can be absorbed by the shape change of the bellows 30. Therefore, damage due to thermal expansion of the connecting cylinder 3 can be prevented, and the stability and safety of the apparatus can be improved. EXAMPLES The invention is further illustrated by the following examples, but the invention is not limited thereto. Example 1 制造 The production of trichlorodecane was carried out using the apparatus for producing trichloromethane shown in Figs. 1 to 3, and it was investigated whether or not the reaction vessel and the extraction tube were deformed or damaged. <Device Description> The following members were used in this device. Reaction vessel: a cylindrical body of a straight cylindrical shape made of an isotropic graphite having an outer diameter of 15 cm, a height of 10 cm, and a thickness of 3 cm. A plurality of outer peripheral surfaces of 3.5 cm from the upper end and 3.5 from the lower end were prepared. The outer peripheral surface of the cm is provided with a carbon-shaped cylindrical body having a male threaded crotch portion. Further, the upper end side of the top cover portion constituting the reaction container and the lower end side of the bottom plate portion constituting the reaction container have a substantially cylindrical shape, and a male screw portion is also provided on the outer peripheral surface of the end portion on the connection side. Further, a raw material gas introduction port having a diameter of 2.5 cm and a height of 10 cm of the tubular projecting portion around the opening is provided in the center of the bottom plate of the substantially cylindrical body at the lower end side, and a substantially cylindrical body disposed above the body portion of the reaction container is provided. A reaction gas extraction port having a diameter of 1.6 cm was provided on the outer peripheral surface. Next, in order to form a tantalum carbide film on the inner circumferential surface and the outer circumference -23-201034954 of the carbon rough cylindrical body, a carbon-made substantially cylindrical body is placed in the CVD reactor, and the inside of the apparatus is replaced with argon gas. To 1200 °C. A mixed gas of trichloromethylnonane and hydrogen (molar ratio 1:5) was introduced into the CVD reactor, and a ruthenium carbide film having a thickness of 200 μm was formed on the entire surface of a substantially cylindrical body made of carbon by a CVD method. Next, a plurality of carbon rings made of isotropic graphite having an inner diameter of 15 cm, a width of 7.5 cm in the vertical direction, and a thickness of 3.6 cm in the radial direction were prepared, and the carbon-shaped ring formed of the above-mentioned carbon was formed on the inner peripheral surface. The carbon ring of the female screw portion of the male screw portion formed by the body is applied to the carbon ring of the female screw portion in the same manner as described above. A reaction vessel is formed by using such a carbon-shaped substantially cylindrical body and a carbon ring. 抽 Extraction pipe: A carbon extraction pipe which is formed by linearly connecting three hollow pipes having flanges at the joint ends is used. In the carbon extraction tube, a tantalum carbide film was applied to the entire surface in the same manner as described above.抽 The assembled extraction tube has a total length of 40 cm and an outer diameter of 3 cm. Bellows: A bellows made of stainless steel with a total length of 11 cm, an inlet diameter of 4 cm, an axial displacement of 5%, and a displacement of 4% perpendicular to the axis. <Assembling of the device> The bottom portion of the heater and the outer cylinder container having the material gas introduction opening portion and the reaction gas extraction opening portion on the outer peripheral surface, respectively, so as to make the tubular projection of the material gas introduction port of the reaction container The raw material gas is introduced into the opening of the outer cylinder container - 24, 2010, 954, and the reaction container is accommodated so that the reaction product gas extraction port of the reaction container and the reaction gas extraction opening of the outer tube container coincide with each other. Next, one end of the extraction pipe is inserted into the reaction gas extraction opening of the outer cylinder container, and is connected to the reaction product gas extraction port of the reaction container, and one end of the bellows is joined to the outer circumference of the extraction pipe, and the other end is joined to the connection cylinder. In the inner circumference, one end of the connection cylinder is connected to the reaction gas extraction opening of the outer cylinder container, and the other end is connected to the reaction product gas introduction opening of the quenching tower.实验 <Experimental conditions> Using the above apparatus, tetrachloromethane was reacted with hydrogen (mole = 1:1) of a material gas at a normal pressure and a reaction temperature of 1100 ° C in a reaction furnace, and a reaction gas was taken out through a suction pipe. The mixture was sent to a quenching tower, and the temperature was adjusted to 2 (TC coolant (20% trichloromethane concentration) for cooling. The temperature of the cooled reaction product gas derived from the quenching tower was 30 °C. <Experimental Results> After the apparatus was continuously operated for 2,000 hours, the apparatus was disintegrated, and the reaction vessel, the extraction pipe, and the connection cylinder were observed. As a result, no deformation or breakage was observed in any of the members. Comparative Example 1 A trichloromethane manufacturing apparatus was adjusted in the same manner as in the above-described Example 1, except that a cylindrical member having a corrugated structure (thickness: 2 mm) was placed instead of the bellows. This tubular member was composed of the same material as that of the bellows used in Example 1, and the joining method of the connecting cylinder or the extracting tube was also carried out in the same manner as in Example 1 -25-10334954. This trichlorodecane was operated in the same manner as in Example 1. In the manufacturing apparatus, the apparatus was disassembled, and the reaction vessel, the extraction pipe, the connection cylinder, and the cylindrical member were observed, and as a result, deformation was observed in the extraction pipe and the tubular member. Comparative Example 2 A flat plate-shaped member (thickness: 2 mm) having an opening through which the extraction pipe can be inserted is used instead of the bellows, and the space on the reactor side and the space on the quenching tower side are blocked in the vicinity of the center of the connection cylinder, In the first embodiment, the apparatus for producing triclosan was adjusted in the same manner. This flat plate-like member is composed of the same material as the bellows used in the embodiment Ο 1. The apparatus for producing trichloromethane was operated in the same manner as in the example 1, and the apparatus was disassembled, and the reaction vessel, the extraction pipe, the connection cylinder, and the flat plate-like member were observed. As a result, deformation was observed in the extraction pipe at the joint portion with the plate-like member. Comparative Example 3 Trichloromethane was adjusted in the same manner as in Example 1 except that the top cover portion of the reaction container was fixed to the ceiling of the outer tube container so as to be fixed to the ceiling portion of the thick outer tube container. In the same manner as in the first embodiment, the temperature of the outer surface of the ceiling portion of the outer cylinder container was increased by 30% as compared with the case of the first embodiment, and the heat of the reaction container was leaked to the outside. Also, the crack was seen in the reaction vessel, and it became impossible to turn around until 2000 hours. <Experimental Investigation> As is apparent from the above comparative experiment, the end of the extraction tube is kept freely by the bellows, and the reaction container is supported by the self-weight only at the bottom of the reaction container only -26-201034954 It can protect the whole device from deformation or damage. Further, since the contact area between the reaction container and the outer tube container is small, leakage of heat from the reaction container to the outside can be suppressed, and the production efficiency of triclosan can be improved. The present invention has been described above on the basis of the examples. This embodiment is exemplified in the end, and it is understood by those skilled in the art that various modifications are possible, and such modifications are also within the scope of the invention. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is an explanatory view showing a device for producing a trichlorosilane according to an embodiment of the present invention. Fig. 2 is a schematic longitudinal cross-sectional view showing the vicinity of a coupling cylinder of a trichloromethane manufacturing apparatus according to an embodiment of the present invention. Fig. 3 is a schematic longitudinal cross-sectional view showing an embodiment of a reaction container usable in the present invention. [Explanation of main component symbols] I Reaction furnace 抽 2 Extraction pipe 3 Connection cylinder 4 Quench tower 10 Reaction vessel II Heater 12 Outer cylinder container Raw material gas introduction port reaction to generate gas extraction port -27- 14 201034954 15 16 18 19 2 1 22 23 Ο 24 25 30 3 1 40 4 1 42 发热 Heating element electrode material gas introduction opening reaction generation gas extraction opening tubular projection 1st member second member third member reaction generation gas ejection portion projection bellows plate metal The reaction of the container to generate gas into the opening is roughly cylindrical ring-28-