.201036913 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 耐熱性優異之三氯矽烷製造裝置。 【先前技術】 三氯矽烷（SiHCl3)係半導體、液晶面板、太陽電池等之 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 〇 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。。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 [Prior Art] Trichloromethane (SiHCl3) is a special material gas used in the manufacture of semiconductors, liquid crystal panels, solar cells, and the like. In recent years, demand has been rapidly expanded, and CVD materials widely used in the field of electronics are expected to grow in the future. Trichloromethane is produced by bringing tetrachlorosilane (SiCl4) into contact with hydrogen (h2) to achieve the following thermal equilibrium state.
SiCl4 + Η2<=» SiHCla + 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〜1 300 °C而進行。 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烷 Ο 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之不同，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、未凝縮氯矽烷，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 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 -4- 201036913 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 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600 °C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。此文獻中提案一種裝置，其具備藉由將四氯 矽烷與氫導入反應室，在600 °C〜1 200 °C的溫度使進行轉 化反應，而得到含三氯矽烷與氯化氫的反應生成氣體後， 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秒以內急冷到3 00 °C以下 爲止的冷卻手段。 又，專利文獻2中記載於經加熱到超過溫度1 200°C且 1400°C以下的反應器中，導入SiCl4與H2的莫耳比爲1:1 〜1:2的混合氣體，使反應而成爲熱平衡狀態（其平衡狀態 的混合物之81(：14與H2的莫耳比爲1:1〜1:4)，再於1秒 以內將含有SiHCl3與HC1等的混合物急冷到6〇0°C以下， 而使反應凍結，提高SiHCl3的收率及收量的siHCl3之製 造法。 201036913 [專利文獻1]特公昭5 7-3 85 24公報 [專利文獻2]特開昭60-81010號公報 【發明內容】 還有，於專利文獻1所記載的裝置中，反應爐與急冷 塔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。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。 〇 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 〇 又，於專利文獻2所記載的裝置中’插入有用於將反 ^ 應生成氣體導出到反應器的排氣側端部之取出管’例如毛 細管或拉瓦爾（Laval)噴管，取出管與反應器的排氣側端部 之接合部係以反應生成氣體不洩漏的方式氣密固定。反應 生成氣體在通過該取出管之際被自然地冷卻。 然而，於上述構成的裝置中，由於反應生成氣體的冷 卻係任憑在通過取出管之際的自然冷卻，故在冷卻速度及 冷卻能力之點未必能說是充分。又，若反應器的排氣側端 部或貫穿其而固定的取出管發生熱膨脹，則對此等的接合 201036913 部施加應力，而會發生變形或破損。 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，其在反應爐與急冷塔的連結部能不發生 熱膨脹所致的變形或破損。更具體地，目的爲提供一種三 氯矽烷製造裝置，在連繫高溫條件下生成反應氣體的反應 爐與將反應氣體冷卻的急冷塔之連結筒，在連結筒內遮斷 反應爐與急冷塔之間的空間之遮斷構件，以及由收納於反 應爐內的反應容器使反應生成氣體通過前述連結筒內導出 至急冷塔的抽出管中，可吸收熱膨脹所發生的應力，同時 減低該熱膨脹所致的應力之發生。 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反應容器、加熱前述反應容器的 加熱器、與收納前述反應容器和加熱器的外筒容器之反應 爐， 將前述反應生成氣體冷卻之急冷塔’ 具備在前述反應爐與急冷塔之間可伸縮連結的第一波紋 管之連結筒， 以由前述反應容器通過前述連結筒內部到達前述急冷塔 的方式所配置，將前述反應生成氣體由反應爐導出到急冷 塔之抽出管，及 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 201036913 外周之第二波紋管。 於此三氯矽烷製造裝置中，藉由具備一種具有連結反 應爐與急冷塔的連結筒爲波紋構造之第一波紋管’於對連 結筒加熱之際，可藉由第一波紋管的形狀變化來吸收熱膨 脹所發生的應力。因此，可防止連結筒之由於熱膨脹所致 的破損，可提高裝置的安定性、安全性。 再者，反應爐內部的空間與急冷塔內部的空間’由於 係被在抽出管和連結筒之間之與彼等大致同軸配置的第二 〇 波紋管所遮斷，故抽出管即使熱膨脹，遮斷手段的第二波 紋管係追隨其而適宜地伸縮，可吸收它。因此，可藉由熱 膨脹來防止抽出管或遮斷手段的破損，可提高裝置的安定 性、安全性，同時可更安定地維持兩塔間的氣密狀態。 又，藉由在反應爐與急冷塔的連結部雙重地配設波紋 管，亦可吸收熱膨脹以外的原因所發生的應力。因此，例 如耐震性亦優異。 再者，由於高溫的外筒容器內之空間與低溫的急冷塔 〇 w 內之空間係被第二波紋管所遮斷，故在該第二波紋管的內 外進行熱交換。於本發明中，由於第二波紋管係在連結筒 內部以覆蓋抽出管的方式大略同軸地配置，故可沿著第二 波紋管自外筒容器側起到急冷塔側爲止，形成溫度緩和下 降的中間溫度區域。結果，對抽出管所施加的熱負荷可在 該區域中廣泛地分散，可防止在抽出管發生局部的大應力 依照本發明的三氯矽烷製造裝置，由於連結反應爐與 201036913 急冷塔的連結筒具備第一波紋管，而且在連結筒內反應爐 與急冷塔係被與抽出管大致同軸配置的第二波紋管所遮斷 ，故在此等部位可防止熱膨脹所致的破損，可提高裝置的 安定性、安全性。 而且，更應大書特寫，依照本發明的三氯矽烷製造裝 置，藉由在連結筒內部以覆蓋抽出管的方式配置第二波紋 管，可在連結筒內部形成中間的溫度區域，而分散對抽出 管所施加的熱負荷，故可防止在抽出管發生局部大的應力 ❹ 【實施方式】 以下，使用圖面來說明本發明的實施形態。尙且’於 所有的圖面中，同樣的構成要素附有同一符號’適宜地省 略說明。 第1圖係示意地顯示本發明的三氯砂院製造裝置之一 實施形態。又，第2圖係示意地顯示該三氯矽烷製造裝置 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砂院與 氯化氫的反應生成氣體之反應容器10、加熱前述反應容器 10的加熱器11、與收納前述反應容器10和加熱器11的 外筒容器12之反應爐1’ 將前述反應生成氣體冷卻之急冷塔4’ 具備在前述反應爐1與急冷塔4之間可伸縮連結的第一 201036913 波紋管30之連結筒3， 以由前述反應容器1〇通過前述連結筒3內部到 冷塔4的方式所配置，將前述反應生成氣體由反j 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 軸地配置，一端接合於連結筒3的內周，另一端 出管2的外周之第二波紋管31。 <反應爐> 〇 反應爐1具備反應容器10、以包圍該反應容蓉 側之方式所配置的長條狀加熱器11、及收納前述 10和加熱器11的外筒容器12。藉由加熱器11 應容器10的外壁，使由反應容器10的底部所設 氣體導入口 13所供給的四氯矽烷與氫之混合氣 容器10內部於約800°c至約1 300°c的高溫反應 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 的略圓筒形狀之容器，具有引進原料氣體的原料 口 13、與用於導出反應生成氣體的反應生成氣 i 4。於本實施形態中，係成爲原料氣體導入口 1 反應容器10的底部中央，反應生成氣體抽出口 反應容器10的上方之側壁的構成，但是此等的 係不受其所限定。 構成反應容器10的材質係氣密性優異的石墨 達前述急 i爐1導 式大略同 接合於抽 I 10的外 反應容器 來加熱反 置的原料 體在反應 ，而生成 境下反應 氣體導入 體抽出口 3設置在 14設置在 設置位置 材，特別 -10- 201036913 地從由於微粒子構造而強度高、熱膨脹等特性對於任一方 向皆相同來看，較佳爲使用耐熱性及耐飩性亦優異的等方 向性高純度石墨。 特別地，較佳爲反應容器1 〇的內周面及/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〜 5 ΟΟμιη的厚度所形成。由於碳化矽被膜對於化學分解具有 極高耐性，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10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 〇 w 碳板、耐火磚、絕熱磚等的絕熱材所被覆的略圓筒形狀之 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，而與後述的連結筒3可能連接 -11- 201036913 <連結筒> 本實施形態的連結筒3具備： 在一端具有連接於反應爐1之反應生成氣體抽出開口部 18的接合手段且在另一端具有經擴徑的收容部34之第一 筒狀構件3 2， 在一端具有插入前述第一筒狀構件32之收容部34側的 插入側端部且在另一端具有連接於急冷塔4的接合手段之 第二筒狀構件3 3，及 〇 收納於前述收容部34，一端固定於第一筒狀構件32的 收容部34側端部，另一端固定於第二筒狀構件33的插入 側端部之第一波紋管3 0。 <第一筒狀構件> 第一筒狀構件32係由不銹鋼等的金屬所構成，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 之凸緣等的接合手段，在另一端具有用於收納第一波紋管 30的收容部34。收容部34係由在第一筒狀構件32的徑 ^ 向外側垂直延伸的直立部35、自該直立部35沿著軸向延 伸的擴徑部36、與由該擴徑部36在徑向內側垂直延伸的 邊緣部3 7所構成。 前述邊緣部37係固定第一波紋管3〇的一端之部位， 邊緣部37之朝徑向內側的突出寬度，係在能固定第一波 紋管30的一端之範圍內，不妨礙第二筒狀構件33的插入 ’而且於不妨礙所插入的第二筒狀構件33在軸向及徑向 自由地移動之範圍。 -12- 201036913 <第二筒狀構件> 第二筒狀構件33係與前述第一筒狀構件32同樣地由 不銹鋼等的金屬所構成，在一端具有用於連接後述的急冷 塔4之反應生成氣體導入開口部45的凸緣等之接合手段 ，在另一端（插入前述第一筒狀構件32的收容部34側之插 入側端部）具有在第二筒狀構件3 3的徑向外側垂直延伸之 凸緣部3 8。 前述凸緣部38係固定第一波紋管30的一端之部位， 〇 凸緣部38之朝徑向外側的突出寬度係在能固定第一波紋 管30的一端之範圍內，不妨礙對第一筒狀構件32的插入 ，而且於插入第一筒狀構件32的狀態下係在不妨礙第二 筒狀構件33在軸向及徑向自由地移動之範圍。 <第一波紋管> 第一波紋管30係具備由金屬所構成的筒狀波紋構造之 構件，在軸心方向能伸縮，同或在徑向亦能變形。此第一 波紋管30係可爲金屬製，更佳爲不銹鋼鋼製，可爲沃斯 Θ 田鐵系不銹鋼鋼製或肥粒鐵系不銹鋼鋼製。 第一波紋管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，較佳爲與 軸垂直方向的位移量係第一波紋管3 0的入口徑之3〜1 0% ，軸向的位移量係全長的2〜5%左右。又’山的間隔或高 度係可爲均一或不均一。 於上述構成的連結筒3中，第一波紋管30係收納於第 —筒狀構件32的收容部34，其兩端分別固定在第一筒狀 -13- 201036913 構件32的邊緣部37及第二筒狀構件33的凸緣部38之相 對面的構成。因此，第一波紋管30在其內側係被第二筒 狀構件33的軀體部所覆蓋。 爲了組裝上述構成的連結筒3，例如可將第一波紋管 30的兩端分別固定在第一筒狀構件32的邊緣部37及第二 筒狀構件33的凸緣部38，在該狀態下將第二筒狀構件33 插入於第一筒狀構件32，將第一波紋管30收納在收容部 34。又’亦可爲在第一筒狀構件32的邊緣部37另途安裝 Θ 相當的構件之構成。 〈急冷塔> 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42、用於將冷卻 液冷卻的冷卻裝置43、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44。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45，在該反應SiCl4 + Η2 <=» SiHCla + HC1 (1) This reaction is carried out by heating a raw material gas composed of vaporized tetrachlorosilane and hydrogen to 800 ° C to 1 300 ° C in a reaction vessel. The high-temperature reaction product gas discharged from the reaction vessel contains a large amount of unreacted tetrachlorodecane ruthenium and hydrogen in addition to the produced trichloromethane and hydrogen chloride. In order to take out trichloromethane from the reaction product gas, a method of condensing in a distillation column using a difference in boiling point between tetrachloromethane and trichloromethane is used. Specifically, in the condenser, the condensed component of chlorodecane is separated from the condensed portion of hydrogen chloride, hydrogen, and non-condensed chlorodecane, and then cooled to about -70 ° C by cryogenic separation to separate from the condensed portion. Trichloromethane. When the desired trichloromethane is separated from the reaction product gas, if the high-temperature reaction product gas immediately after the reaction vessel is suddenly introduced into the distillation column, an excessive load is applied to the distillation column, so that it is typically Anti-4-201036913 Before the gas should be introduced into the distillation column, it must be pre-cooled in the quenching tower. 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 instantaneously cool the reaction product gas to a predetermined temperature and freeze the equilibrium at the time when the balance is sufficiently reached on the trichloromethane side. In order to instantaneously freeze the above equilibrium state, 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. In this document, a device is proposed which comprises introducing tetrachlorosilane and hydrogen into a reaction chamber, and performing a conversion reaction at a temperature of from 600 ° C to 1 200 ° C to obtain a reaction gas containing trichloromethane and hydrogen chloride. A cooling means for causing contact with a mixture of chlorodecane cooled to room temperature by a reaction gas derived from a reaction chamber, and quenching to 300 ° C or less within 1 second. Further, in Patent Document 2, a mixed gas in which a molar ratio of SiCl4 and H2 is 1:1 to 1:2 is introduced into a reactor heated to a temperature exceeding 1 200 ° C and 1400 ° C or lower to cause a reaction. Became a thermal equilibrium state (the mixture of 81 in equilibrium) (the molar ratio of 14 to H2 is 1:1 to 1:4), and then quench the mixture containing SiHCl3 and HC1 to 6 〇 0 ° C within 1 second. In the following, a method of producing siHCl 3 which is used to freeze the reaction and increase the yield and yield of SiHCl 3 is disclosed. [Patent Document 1] Japanese Patent Publication No. 5-7-3 85-24 [Patent Document 2] JP-A-60-81010 Further, in the apparatus described in Patent Document 1, the reaction furnace and the quenching tower are connected via a connecting pipe provided on the side of the quenching tower to form a closed end portion at the joint portion between the connecting pipe and the reaction furnace. Passing the probe through the closed end, the reaction gas generated by the reaction furnace is led to the quenching chamber through the probe. However, the high temperature reaction furnace and the low temperature quenching chamber are connected to the reaction furnace The closed end wall of the joint is covered by the shadow A large local temperature difference occurs between the end wall surface of the reactor and the vicinity of the reactor. As a result, the stress caused by the thermal expansion concentrates on the portion and deforms or breaks. Further, the probe fixed through the end wall surface also thermally expands. In the apparatus described in Patent Document 2, the junction portion of the probe and the end wall surface is concentrated, and the exhaust side portion for introducing the reaction product gas to the reactor is inserted. The take-out pipe 'for example, a capillary or a Laval nozzle, and the joint portion of the take-out pipe and the exhaust side end portion of the reactor is hermetically fixed in such a manner that the reaction gas does not leak. The reaction gas is passed through the take-up pipe. However, in the apparatus having the above configuration, since the cooling system of the reaction product gas is naturally cooled by the removal of the tube, it is not necessarily sufficient at the point of cooling rate and cooling capacity. If the exhaust side end of the reactor or the take-out tube fixed therethrough thermally expands, stress is applied to the joint 201036913, and deformation occurs. The present invention has been made in view of the above circumstances, and an object thereof is to provide a device for producing triclosan which is capable of deformation or breakage due to thermal expansion at a joint portion between a reaction furnace and a quenching tower. More specifically, the object is to provide A device for manufacturing a trichloromethane, a connecting member for a reaction furnace for generating a reaction gas under a high temperature condition and a quenching tower for cooling the reaction gas, and a blocking member for interrupting a space between the reaction furnace and the quenching tower in the connecting cylinder And the reaction product gas is taken out into the extraction pipe of the quenching tower through the reaction vessel housed in the reaction furnace, thereby absorbing the stress generated by the thermal expansion and reducing the stress caused by the thermal expansion. In order to solve the aforementioned problems, the following constitution is adopted. In other words, the apparatus for producing a trichloromethane of the present invention includes a reaction vessel that generates a reaction gas containing trichloromethane and hydrogen chloride from a raw material gas containing tetrachlorosilane and hydrogen, and a heater that heats the reaction vessel. a quenching furnace for cooling the reaction-generating gas with a reaction furnace for accommodating the outer cylinder container of the reaction vessel and the heater, and a connecting tube of the first bellows that is expandably coupled between the reaction furnace and the quenching tower, The reaction container is disposed such that the inside of the connecting cylinder reaches the quenching tower, and the reaction product gas is led out from the reaction furnace to the extraction pipe of the quenching tower, and the inside of the connecting cylinder is disposed substantially coaxially so as to cover the extraction pipe. One end is joined to the inner circumference of the coupling cylinder and the other end is joined to the second bellows of the outer circumference of the 201036913 of the extraction pipe. In the apparatus for producing trichloromethane, the first bellows having a corrugated structure having a connecting cylinder connecting the reaction furnace and the quenching tower can be heated by the first corrugated tube, and the shape of the first bellows can be changed. To absorb the stress that occurs when thermal expansion occurs. Therefore, damage to the connecting cylinder due to thermal expansion can be prevented, and the stability and safety of the device can be improved. Further, since the space inside the reaction furnace and the space inside the quenching tower are blocked by the second 〇 bellows disposed between the extraction pipe and the connecting cylinder and substantially coaxial with each other, the extraction pipe is thermally expanded even. The second bellows of the breaking means is adapted to flexibly follow it and absorb it. Therefore, the expansion of the extraction pipe or the interruption means can be prevented by thermal expansion, the stability and safety of the apparatus can be improved, and the airtight state between the two towers can be maintained more stably. Further, by providing the bellows in a double connection between the reaction furnace and the quenching tower, it is possible to absorb stress generated by causes other than thermal expansion. Therefore, for example, the shock resistance is also excellent. Further, since the space inside the high-temperature outer cylinder container and the space in the low-temperature quenching tower 〇 w are blocked by the second bellows, heat exchange is performed inside and outside the second bellows. In the present invention, since the second bellows is disposed substantially coaxially so as to cover the extraction pipe inside the connecting cylinder, the temperature can be lowered and lowered along the second bellows from the outer cylinder side to the quenching tower side. Intermediate temperature zone. As a result, the heat load applied to the extraction pipe can be widely dispersed in the region, and local large stress can be prevented from occurring in the extraction pipe. The apparatus for manufacturing a trichloromethane according to the present invention is connected to the quenching tower of the 201036913 quenching tower. The first bellows is provided, and in the connecting cylinder, the reaction furnace and the quenching tower are blocked by the second bellows disposed substantially coaxially with the extraction pipe, so that damage due to thermal expansion can be prevented at these portions, and the device can be improved. Stability and safety. Further, in the case of the apparatus for manufacturing triclosan according to the present invention, by arranging the second bellows so as to cover the extraction tube inside the connection cylinder, an intermediate temperature region can be formed inside the connection cylinder, and the dispersion pair Since the heat load applied to the tube is extracted, it is possible to prevent a local large stress from being generated in the extraction tube. [Embodiment] Hereinafter, an embodiment of the present invention will be described using the drawings. In the drawings, the same components are denoted by the same reference numerals, and the description is omitted as appropriate. Fig. 1 is a view schematically showing an embodiment of the apparatus for producing triclosan of the present invention. Further, Fig. 2 is a view schematically showing a cross section of the periphery of the connecting cylinder of the apparatus for producing triclosan. In the apparatus for producing a trichloromethane of the present embodiment, as shown in Fig. 1 and Fig. 2, a reaction gas for generating a gas containing trichlorosilane and hydrogen chloride is produced by using a raw material gas containing tetrachlorosilane and hydrogen. The reaction vessel 10, the heater 11 for heating the reaction vessel 10, and the reaction furnace 1' for the outer cylinder vessel 12 in which the reaction vessel 10 and the heater 11 are housed, and the quenching tower 4' for cooling the reaction product gas are provided in the reactor a connecting cylinder 3 of the first 201036913 bellows 30 that is telescopically coupled to the quenching tower 4 is disposed by the reaction vessel 1〇 passing through the inside of the connecting cylinder 3 to the cooling tower 4, and the reaction generating gas is The extraction pipe 2 is discharged to the quenching tower 4, and the inside of the connecting cylinder 3 is disposed so as to cover the square shaft of the extraction pipe 2, and one end is joined to the inner circumference of the connection cylinder 3, and the other end is the outer circumference of the outlet tube 2. Two bellows 31. <Reaction Furnace> The reactor 1 includes a reaction vessel 10, a long heater 11 disposed to surround the reaction chamber side, and an outer cylinder container 12 in which the 10 and the heater 11 are housed. The inside of the mixed gas container 10 of tetrachlorosilane and hydrogen supplied from the gas introduction port 13 provided at the bottom of the reaction vessel 10 by the heater 11 in the outer wall of the container 10 is at about 800 ° C to about 1 300 ° C. The high temperature reaction contains a reaction gas of trichloromethane and hydrogen chloride to form a gas. <Reaction vessel> ^ The reaction vessel 10 is a container having a substantially cylindrical shape in which tetrachlorosilane and hydrogen are in a high temperature ring, and has a raw material port 13 into which a raw material gas is introduced, and a reaction product gas for deriving a reaction product gas. 4. In the present embodiment, the raw material gas introduction port 1 is located at the center of the bottom of the reaction container 10, and the reaction generates a side wall above the gas extraction reaction container 10. However, these are not limited thereto. The material constituting the reaction vessel 10 is made of a graphite having excellent airtightness, and the raw material of the first reactor is connected to the outer reaction vessel of the pump I 10 to heat the reversed raw material, thereby generating a gaseous reaction gas introduction body. The suction port 3 is provided at 14 for setting the position material, and in particular, the frequency of the high-intensity, thermal expansion, etc. due to the fine particle structure is the same in any direction, and it is preferable to use heat resistance and stagnation resistance. Isometric high purity graphite. In particular, it is preferred that the inner peripheral surface and/or the outer peripheral surface of the reaction vessel 1 are treated with a tantalum carbide film formed by a CVD method at a thickness of 10 to 5 μm. 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 ruthenium 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 in a plurality, and the temperature inside the reaction vessel 10 is adjusted from the outside of the reaction vessel 10 by controlling the amount of supplied electric power. <Outer tube container> The outer tube container 1 2 is a container having a substantially cylindrical shape 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 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-generating 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. -11 - 201036913 < Connecting cylinder> The connecting cylinder 3 of the present embodiment includes: The reaction of the reaction furnace 1 generates a joining means for the gas extraction opening 18, and has a first cylindrical member 3 2 having an enlarged diameter accommodating portion 34 at the other end, and has an accommodating portion 34 inserted into the first cylindrical member 32 at one end. The second insertion-side end portion on the side and the second cylindrical member 3 3 connected to the joint means of the quenching tower 4 at the other end, and the accommodating portion 34 are accommodated in the accommodating portion 34, and one end is fixed to the accommodating portion 34 of the first cylindrical member 32. The side end portion is fixed to the first bellows 30 of the insertion side end portion of the second cylindrical member 33 at the other end. <First cylindrical member> The first tubular member 32 is made of a metal such as stainless steel, and has a joining means at one end that can be connected to the flange of the reaction product gas extraction opening portion 18 of the outer cylinder container 12, and the like. At the other end, there is a housing portion 34 for accommodating the first bellows 30. The accommodating portion 34 is an upright portion 35 that vertically extends outward in the radial direction of the first tubular member 32, an enlarged diameter portion 36 that extends in the axial direction from the upright portion 35, and a radial direction from the enlarged diameter portion 36. The inner side vertically extends the edge portion 37. The edge portion 37 fixes a portion of one end of the first bellows 3〇, and the protruding width of the edge portion 37 toward the radially inner side is within a range in which one end of the first bellows 30 can be fixed, and does not interfere with the second cylindrical shape. The insertion of the member 33 does not hinder the range in which the inserted second cylindrical member 33 is freely movable in the axial direction and the radial direction. -12-201036913 <Second tubular member> The second tubular member 33 is made of a metal such as stainless steel similarly to the first tubular member 32, and has a quenching tower 4 to be connected to one end at one end. The joining means such as the flange of the reaction-generating gas introduction opening 45 is formed in the radial direction of the second cylindrical member 33 at the other end (the insertion-side end portion inserted into the accommodating portion 34 side of the first cylindrical member 32). The flange portion 38 extends vertically outward. The flange portion 38 fixes a portion of one end of the first bellows 30, and the protruding width of the flange portion 38 toward the radially outer side is within a range in which one end of the first bellows 30 can be fixed, and does not hinder the first The insertion of the tubular member 32 is in a range in which the second cylindrical member 33 is freely moved in the axial direction and the radial direction without being hindered in the state in which the first tubular member 32 is inserted. <First bellows> The first bellows 30 is a member having a cylindrical corrugated structure made of metal, and is expandable and contractible in the axial direction, and can be deformed in the same direction in the radial direction. The first bellows 30 may be made of metal, more preferably stainless steel, and may be made of Worth iron or stainless steel. The first bellows 30 is preferably 2 to 10% of the height of the mountain entrance, and the interval between the mountain and the mountain is about 2 to 8%. Further, it is preferable that the displacement amount in the direction perpendicular to the axis is 3 to 10% of the entrance diameter of the first bellows 30, and the displacement amount in the axial direction is about 2 to 5% of the total length. Also, the spacing or height of the mountain may be uniform or non-uniform. In the connecting cylinder 3 having the above configuration, the first bellows 30 is housed in the accommodating portion 34 of the first tubular member 32, and both ends thereof are fixed to the edge portion 37 of the first cylindrical member-13-201036913 member 32 and The configuration of the opposing surface of the flange portion 38 of the two tubular members 33. Therefore, the first bellows 30 is covered on the inner side by the body portion of the second cylindrical member 33. In order to assemble the connection tube 3 having the above configuration, for example, both ends of the first bellows 30 can be fixed to the edge portion 37 of the first cylindrical member 32 and the flange portion 38 of the second cylindrical member 33, in this state. The second tubular member 33 is inserted into the first tubular member 32, and the first bellows 30 is housed in the accommodating portion 34. Further, a configuration may be adopted in which the member of the first cylindrical member 32 is attached to the edge portion 37 of the first tubular member 32. <Quench Tower> The quenching tower 4 includes a cylindrical metal container 40, a nozzle 41 that sprays a coolant in the container provided in the container, and a coolant that is taken out from the bottom of the container and circulated to the nozzle 41. The pump 42 is provided with a cooling device 43 for cooling the cooling liquid, and a conduit 44 for taking out the cooled reaction product gas from the top of the quenching tower 4. In the side wall of the quenching tower 4, a reaction product gas introduction opening portion 45 for connecting the connection cylinder 3 is provided, in the reaction
D 生成氣體導入開口部45設有用於與連結筒3連接的凸緣 等接合手段。噴嘴41係以能向導入急冷塔4的反應生成 氣體噴灑冷卻液的方式，設置在反應生成氣體導入開口部 45的上部附近。 冷卻液係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8 5 : 1 5、溫度係4 0 °C左右者。 -14- 〇The D-forming gas introduction opening portion 45 is provided with a joining means such as a flange for connecting to the connecting cylinder 3. The nozzle 41 is provided in the vicinity of the upper portion of the reaction product gas introduction opening portion 45 so that the coolant can be sprayed onto the reaction product gas introduced into the quenching tower 4. The cooling liquid is composed of a mixture of trichloromethane and tetrachlorosilane, and the ratio of tetrachlorosilane is 1 to 0.5 with respect to the total amount of tetrachlorosilane and trichlorosilane. The temperature is preferably 60 ° C or less. For example, it is preferred to use a composition ratio of tetrachlorosilane:trichlorosilane of 8 5 : 15 and a temperature of about 40 °C. -14- 〇
201036913 由急冷塔4的頂部所取出的冷卻後之反應生 經由導管44再送到蒸餾塔（未圖示），而進行目的 院的分離。 <抽出管> 抽出管2碳製管狀構件，其通過連結筒3內音f 反應容器10內部與急冷塔4內部，將反應容器1〇 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， 從由於微粒子構造而強度高、熱膨脹等特性對於任 皆相同來看，較佳爲使用耐熱性及耐蝕性亦優異的 性高純度石墨。 特別地，較佳爲抽出管2的內周面及/或外周酉 化矽被膜處理，該碳化矽被膜係藉由CVD法以10' 的厚度所形成。由於碳化矽被膜對於化學分解具窄 性，故可防止碳組織的化學浸蝕。因此，藉由施3 被膜處理，可保護抽出管2的表面防止腐蝕。201036913 The cooled reaction taken out from the top of the quenching tower 4 is sent to a distillation column (not shown) via a conduit 44 to separate the target. <Extraction Tube> The tubular member of the carbon tube 2 is taken out, and the inside of the reaction vessel 10 and the inside of the quenching tower 4 are connected to each other through the internals of the cylinder 3, and the reaction gas is discharged to the quenching tower 4. The material constituting the extraction tube 2 is a high-purity graphite which is excellent in heat resistance and corrosion resistance, and is excellent in properties such as high strength and thermal expansion from the viewpoint of the fine particle structure. In particular, it is preferable that the inner peripheral surface of the extraction tube 2 and/or the outer peripheral ruthenium ruthenium film is formed by a CVD method at a thickness of 10'. Since the tantalum carbide film is narrow in chemical decomposition, chemical etching of the carbon structure can be prevented. Therefore, by applying the film treatment, the surface of the extraction tube 2 can be protected from corrosion.
抽出管2從氣密性或強度之點優異來看，較fg 一的構件所構成，但是亦可連結有複數的構件者。 形態的抽出管2係由複數的構件所構成，在將裝種 際，係由主要位於反應爐1內的第一構件21、主I 結筒3內的第二構件22及主要位於冷卻塔內的負 23所構成。即，第一構件21係在一端具有與反應 的反應生成氣體抽出口 14之連接部，在另一端I 連結第二構件22的接合手段，第二構件22係在P 氣體係 三氯矽 而連繫 內的反 特別地 一方向 等方向 係經碳 -5 0 0 μιη 極高耐 碳化矽 係由單 本實施 :組裝之 :位於連 ;三構件 容器10 有用於 ί端具有 -15- 201036913 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。 抽出管2的接合手段係以接合後述的第二波紋管31之 方式，在抽出管2的外周側形成突出部25者。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，環係形成用於固定第二波紋管3 1 〇 的突出部25。 <第二波紋管> 第二波紋管31係由金屬所構成的波紋構造之構件，在 軸心方向能伸縮，同時在徑向亦能變形。與第一波紋管3 0 同樣地，此第二波紋管31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。 又，可爲單層或多層，較佳爲多層構造的情況，因爲增加 耐腐蝕性。 〇 ^ 第二波紋管31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，較佳爲與 軸垂直方向的位移量係第二波紋管31的入口徑之3〜10% ，軸向的位移量係全長的2〜5%左右。又，山的間隔或高 度係可爲均一或不均一。 第二波紋管31係在連結筒3內部以覆蓋抽出管2的外 側之方式大致同軸配置，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。 -16- 201036913 於本實施形態中，第二波紋管31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的第一筒狀構件32所設 置的接合手段之間夾入甜甜圈狀的板材39，在該板材39 突出連結筒3內的部分固定第二波紋管31的一端而進行 。又’第二波紋管31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與第三構件23的連結部所形 成的突出部25固定第二波紋管31的一端而進行。 Ο 如此地，反應爐1內部的空間與急冷塔4內部的空間 係被連結筒3內配置的第二波紋管31所遮斷。 於本實施形態中，由於以伸縮自在的第一波紋管30來 連接構成連結筒3的構件，故即使在連結筒3有局部的大 溫度差而使第一筒狀構件32及第二筒狀構件33熱膨脹， 藉由第一波紋管30的形狀變化，可吸收與連結筒3有關 的應力，可避免連結筒3的變形或破損。 又，由於第一波紋管30的外側係被第一筒狀構件32 ^ 的擴徑部3 6所覆蓋，內側係被第二筒狀構件3 3的軀體部 所覆蓋，故可防止連結筒3內部所可存在的化學物質，即 反應生成氣體或冷卻液中所含有的反應性物質附著於第一 波紋管30，使其劣化而損害伸縮性。 還有，作爲在連結筒3內周與抽出管2外周之間所連 接的遮斷反應爐1內部的空間與急冷塔4內部的空間之手 段，藉由使用可伸縮的第二波紋管31 ’即使抽出管2進行 熱膨脹或收縮，第二波紋管31也能追隨其而適宜伸縮’ -17- 201036913 故不損害抽出管2，亦不破壞兩空間的遮斷狀態。 再者’由於第二波紋管31係在連結筒3內部以覆蓋抽 出管2方式大略同軸地配置，故可沿著第二波紋管31自 外筒容器側1 2起到急冷塔4側爲止，形成溫度緩和下降 的中間溫度區域。結果，施加於抽出管2的熱負荷可在該 區域中廣泛地分散，可防止在抽出管2發生局部的大應力 〇 而且’本發明的技術範圍係不受上述實施形態所限定 D ，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 本來較佳爲一體成型，但是由於製造技術上的問題，使用 略圓筒體以複數連結一體化者。作爲略圓筒體以複數連結 一體化的反應容器，特別地較佳爲將複數的略圓筒體以端 部彼此對接而大略同軸地上下配置，由外側以環來螺合締 結對接端部者。藉由成爲如此的構造，由於可使略圓筒體 的構造成爲單純者，在上端或下端形成壁厚爲薄的部位， D 故對於物理的衝撃具有優異的耐性。又，由於不是在連結 部中一方的略圓筒體之端部嵌合於另一方的略圓筒體之端 部般的構成’故即使在高溫環境下使用而使略圓筒體進行 熱膨脹，也不會引起由於各個略圓筒體的熱膨脹係數之不 同所致的連結部之破裂或龜裂。因此，可減低交換反應容 器的構成構件之頻率，改善裝置的作業效率。 又’於上述實施態樣中，將第一波紋管收納在第一筒 狀構件的收容部’將其內側以第二筒狀構件的軀體部覆蓋 -18- 201036913 而構成，但若於第一筒狀構件與第二筒狀構件的連結部使 用第一波紋管，則可充分吸收對連結筒所施加的應力，第 一波紋管亦可收納在第一筒狀構件與第二筒狀構件之間。 還有，於上述實施態樣中，將第二波紋管的反應爐側 端部連接於連結筒，將急冷塔側端部連接於抽出管而構成 ，但亦可與此相反地連接。即，第二波紋管與連結筒內側 的連接，係可藉由在外筒容器的急冷塔之反應生成氣體導 入開口部所設置的接合手段與在連結筒的第二筒狀構件所 設置的接合手段之間夾入甜甜圈狀的板材1在該板材突出 連結筒內的部分固定第二波紋管的一端而進行，第二波紋 管與抽出管外側的連接，係藉由在構成抽出管的第一構件 與第二構件的連結部所形成的突出部固定第二波紋管的一 端而進行。 再者，於上述實施態樣中，抽出管係由3個構件所構 成’但是亦可由單一的構件所構成，或可由更多的構件所 構成。 Θ 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 使用第2圖所示的三氯矽烷製造裝置來進行三氯矽烷 的製造’調查連結筒、抽出管及第二波紋管有無變形或破 損。 <裝置說明> -19- 201036913 於此裝置中使用以下的構件。 連結筒： 使用經由不錄鋼鋼製的波紋管（厚度：2mm)連結有不绣 鋼製的筒狀構件之連結筒。此波紋管之與軸垂直方向的位 移量係入口徑的5 %左右’軸向的位移量係全長的5 %左右 〇 第二波紋管： 使用不銹鋼鋼製的波紋管。此波紋管之與軸垂直方向 ^ 的位移量係入口徑的5 %左右，軸向的位移量係全長的5 % 左右。 抽出管： 使用施有碳化矽被膜處理的碳製管狀構件。 <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，使用溫度經調節20 〇 w °C的冷卻液（三氯矽烷濃度20%)來冷卻。 連續地運轉此三氯矽烷製造裝置2000小時後，將裝置 解體，觀察連結筒、抽出管及第二波紋管，結果在任一構 件皆沒有觀察到變形或破損。 比較例1 除了代替第二波紋管，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使用的第二波紋管相 -20- 201036913 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，觀察連結筒、抽出管及筒狀構件，結果在抽出管與 筒狀構件看到變形。 比較例2 除了代替第二波紋管，使用具有抽出管可貫穿的開口 之板狀構件（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。此筒狀構件係由與實施例1使 用的第二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，觀察連結筒、抽出管及板狀構件，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 除了代替連結筒，配設沒有第一波紋管的筒狀構件（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使用的連結筒之第一和 第二筒狀構件相同的材質所構成。 與實施例1同樣地運轉此三氯矽烷製造裝置，將裝置 解體，觀察裝置筒狀構件、抽出管及第二波紋管，結果在 筒狀構件看到變形。 <實驗的考察> 如由以上的比較實驗可明知，連接反應爐與急冷塔的 連結筒係具備第一波紋管，而且反應爐與急冷塔係被在抽 -21- 201036913 出管與連結筒之間配設的第二波紋管所遮斷，藉由此構成 ，可防止熱膨脹所致的此等構件之變形或破損，可提高裝 置的安定性、安全性。又，藉由在連結筒內部以覆蓋抽出 管的方式配置第二波紋管，可分散對抽出管所施加熱負荷 ，可防止在抽出管發生局部的大應力。 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，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。 〇 【圖式簡單說明】 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。 【主要元件符號說明】 1 2The extraction pipe 2 is formed of a member of the fg one from the viewpoint of excellent airtightness or strength, but may be connected to a plurality of members. The form of the extraction pipe 2 is composed of a plurality of members, and is installed in the first member 21 mainly located in the reaction furnace 1, the second member 22 in the main I-cylinder 3, and mainly located in the cooling tower. The negative 23 is composed. That is, the first member 21 is a joining means having a connection portion with the reaction reaction product gas discharge port 14 at one end, and a second member 22 is connected to the other end I, and the second member 22 is connected to the P gas system trichloroantimony. The anti-special direction in the system is in the same direction as the carbon-5 0 0 μιη extremely high carbonization resistant lanthanide system by a single implementation: assembly: located in the joint; three-component container 10 has been used for ί-end with -15-201036913 The joining means for joining the first member 21 or 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. 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 second bellows 31 to be described later. As the joining means for forming such a projection 25, a flange can be typically used. Further, a tubular member having a substantially cylindrical shape may be used, and the end portion of the butt joint may be screwed and joined by a ring from the outside. In this case, the ring system forms a projection 25 for fixing the second bellows 3 1 〇. <Second bellows> The second bellows 31 is a member having a corrugated structure made of metal, which is expandable and contractible in the axial direction and deformable in the radial direction. Similarly to the first bellows 30, the second bellows 31 may be made of metal, more preferably stainless steel, and may be made of Worthite iron-based stainless steel or fat-coated iron-based stainless steel. Further, it may be a single layer or a plurality of layers, preferably in the case of a multilayer structure because of increased corrosion resistance. 〇 ^ The second bellows 31 is preferably 2 to 10% of the height of the mountain entrance, and the interval between the mountain and the mountain is about 2 to 8%. Further, it is preferable that the displacement amount in the direction perpendicular to the axis is 3 to 10% of the entrance diameter of the second bellows 31, and the displacement amount in the axial direction is about 2 to 5% of the total length. Also, the spacing or height of the mountains may be uniform or non-uniform. The second bellows 31 is disposed substantially coaxially inside the connecting tube 3 so as to cover the outer side of the drawing tube 2, and one end is joined to the inner circumference of the connecting tube 3, and the other end is joined to the outer circumference of the drawing tube 2. -16- 201036913 In the present embodiment, the connection between the second bellows 31 and the inner circumference of the connection cylinder 3 is formed by the engagement means provided in the reaction of the outer cylinder container 12 to generate the gas extraction opening 18 and the connection cylinder 3. A donut-shaped plate member 39 is interposed between the joining means provided in the first tubular member 32, and a portion of the plate member 39 that projects into the connecting tube 3 is fixed to one end of the second bellows 31. Further, the connection between the second bellows 31 and the outer circumference of the extraction pipe 2 is one end of the second bellows 31 fixed by the projection 25 formed at the joint portion of the second member 22 and the third member 23 constituting the extraction pipe 2. And proceed. In this manner, the space inside the reaction furnace 1 and the space inside the quenching tower 4 are blocked by the second bellows 31 disposed in the connecting cylinder 3. In the present embodiment, since the member constituting the connecting cylinder 3 is connected to the first bellows 30 that is stretchable and contractible, the first cylindrical member 32 and the second tubular shape are formed even if there is a large temperature difference in the connecting cylinder 3 The member 33 is thermally expanded, and the stress associated with the connecting cylinder 3 can be absorbed by the shape change of the first bellows 30, and deformation or breakage of the connecting cylinder 3 can be avoided. Further, since the outer side of the first bellows 30 is covered by the enlarged diameter portion 36 of the first tubular member 32^ and the inner portion is covered by the body portion of the second cylindrical member 33, the connection cylinder 3 can be prevented. The chemical substance that can be present inside, that is, the reaction product gas or the reactive substance contained in the cooling liquid adheres to the first bellows 30, and deteriorates to impair the stretchability. Further, as a means for blocking the space inside the reactor 1 and the space inside the quenching tower 4 connected between the inner circumference of the connecting cylinder 3 and the outer circumference of the extraction pipe 2, by using the second bellows 31' which is retractable Even if the extraction pipe 2 is thermally expanded or contracted, the second bellows 31 can follow it and is suitable for expansion and contraction -17-201036913, so that the extraction pipe 2 is not damaged, and the interruption state of both spaces is not damaged. In addition, since the second bellows 31 is disposed substantially coaxially inside the connecting cylinder 3 so as to cover the extraction pipe 2, the second bellows 31 can be moved from the outer cylinder container side 1 to the quenching tower 4 side along the second bellows 31. An intermediate temperature region where the temperature is moderately lowered is formed. As a result, the heat load applied to the extraction pipe 2 can be widely dispersed in the region, and local stress can be prevented from occurring locally in the extraction pipe 2, and the technical scope of the present invention is not limited to the above-described embodiment D. Various changes 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 is preferably integrally molded, but due to manufacturing problems, a plurality of integrated bodies are used in a plurality of cylinders. In particular, it is preferable that a plurality of substantially cylindrical bodies are integrally connected to each other with a plurality of substantially cylindrical bodies that are butt-joined at the ends, and that the abutting ends are screwed and joined by a ring from the outside. . With such a structure, since the structure of the substantially cylindrical body can be made simple, a portion having a thin thickness is formed at the upper end or the lower end, so that D has excellent resistance to physical punching. In addition, since the end portion of the slightly cylindrical body of one of the joint portions is not fitted to the end portion of the other slightly cylindrical body, the cylindrical body is thermally expanded even when used in a high-temperature environment. It also does not cause cracking or cracking of the joint due to the difference in thermal expansion coefficient of each of the slightly cylindrical bodies. Therefore, the frequency of the constituent members of the exchange reaction container can be reduced, and the work efficiency of the apparatus can be improved. Further, in the above-described embodiment, the first bellows is housed in the accommodating portion ' of the first tubular member, and the inner portion thereof is covered with the body portion of the second tubular member -18-201036913, but if it is first When the first bellows is used in the joint portion between the tubular member and the second tubular member, the stress applied to the joint cylinder can be sufficiently absorbed, and the first bellows can be accommodated in the first tubular member and the second tubular member. between. Further, in the above embodiment, the reactor-side end portion of the second bellows is connected to the connection cylinder, and the quenching tower-side end portion is connected to the extraction tube. However, the opposite side may be connected. That is, the connection between the second bellows and the inside of the connecting cylinder is a joining means provided by the reaction of the quenching tower of the outer cylinder container to form the gas introduction opening and the second cylindrical member of the connecting cylinder. The sheet 1 sandwiching the donut-shaped plate is formed by fixing one end of the second bellows in a portion of the plate protruding connection cylinder, and the connection between the second bellows and the outer side of the extraction tube is by the first portion constituting the extraction tube The protruding portion formed by the connecting portion of the one member and the second member is fixed by fixing one end of the second bellows. Further, in the above embodiment, the extraction pipe system is composed of three members', but may be composed of a single member or may be composed of more members. EXAMPLES The present invention will be further illustrated by the following examples, but the present invention is not limited thereto. Example 1 The production of trichloromethane was carried out using the apparatus for producing triclosan shown in Fig. 2 to investigate whether the connecting cylinder, the extraction pipe and the second bellows were deformed or damaged. <Device Description> -19- 201036913 The following components were used in this apparatus. Connecting cylinder: A connecting cylinder of a cylindrical member made of stainless steel is connected to a bellows (thickness: 2 mm) made of non-recorded steel. The amount of displacement of the bellows in the direction perpendicular to the axis is about 5% of the diameter of the inlet. The amount of displacement in the axial direction is about 5% of the total length. 〇 Second bellows: Bellows made of stainless steel. The displacement of the bellows perpendicular to the axis ^ is about 5% of the inlet diameter, and the axial displacement is about 5% of the total length. Extraction tube: A carbon tubular member treated with a tantalum carbide coating. <Experimental Conditions> Using the apparatus described above, tetrachloromethane was reacted with a hydrogen (mole = 1:1) raw material gas at a normal pressure and a reaction temperature of 1,100 ° C in a reaction furnace, and a reaction was taken out through a withdrawal tube. The gas is sent to a quenching tower and cooled using a coolant (20% trichloromethane concentration) adjusted to a temperature of 20 〇 w °C. After the apparatus for manufacturing the trichloromethane was continuously operated for 2,000 hours, the apparatus was disassembled, and the connecting cylinder, the extraction tube, and the second bellows were observed, and as a result, no deformation or breakage was observed in any of the members. Comparative Example 1 A trichlorodecane production apparatus was adjusted in the same manner as in the above-described first embodiment, except that a tubular member having a corrugated structure (thickness: 2 mm) was disposed instead of the second bellows. This cylindrical member is composed of the same material as the second bellows -20-201036913 used in the first embodiment. The apparatus for producing triclosan was operated in the same manner as in the first embodiment, and the apparatus was disassembled, and the connecting cylinder, the extraction tube, and the tubular member were observed. As a result, the extraction tube and the tubular member were deformed. Comparative Example 2 In place of the second bellows, a plate-like member (thickness: 2 mm) having an opening through which the extraction pipe can be inserted is used, and the space on the reaction furnace side and the space on the quenching tower side are blocked in the vicinity of the center of the connection cylinder, In the above-described first embodiment, the apparatus for producing triclosan was adjusted in the same manner. This cylindrical member is composed of the same material as that of the second bellows used in the first embodiment. The apparatus for producing triclosan was operated in the same manner as in the first embodiment, and the apparatus was disassembled, and the connecting cylinder, the extraction tube, and the plate-like member were observed. As a result, deformation was observed in the extraction tube at the joint portion with the plate-like member. Comparative Example 3 A trichlorodecane production apparatus was adjusted in the same manner as in the above-described first embodiment except that a cylindrical member (thickness: 2 mm) having no first bellows was disposed instead of the connection cylinder. This cylindrical member is composed of the same material as the first and second cylindrical members of the connecting cylinder used in the first embodiment. The apparatus for producing trichloromethane was operated in the same manner as in the first embodiment, and the apparatus was disassembled, and the tubular member, the extraction tube, and the second bellows were observed, and as a result, deformation was observed in the tubular member. <Experimental Investigation> As can be seen from the above comparative experiments, the connecting cylinder connecting the reaction furnace and the quenching tower is provided with the first bellows, and the reaction furnace and the quenching tower are taken out and connected at -21,369,139,313 The second bellows disposed between the cylinders is blocked, whereby the deformation or breakage of the members due to thermal expansion can be prevented, and the stability and safety of the device can be improved. Further, by arranging the second bellows so as to cover the extraction pipe inside the connection cylinder, it is possible to disperse the heat load applied to the extraction pipe, and it is possible to prevent local large stress from occurring in the extraction pipe. The present invention has been described above on the basis of the examples. This embodiment is exemplified by 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 the apparatus for producing triclosan in the embodiment of the present invention. [Main component symbol description] 1 2
4 10 11 12 13 14 15 反應爐 抽出管 連結筒 急冷塔 反應容器 加熱器 外筒容器 原料氣體導入口 反應生成氣體抽出口 發熱體 -22- 2010369134 10 11 12 13 14 15 Reactor Furnace extraction tube Connection tube Quench tower Reaction vessel Heater Outer tube container Raw material gas inlet Reaction gas extraction outlet Heating element -22- 201036913
16 電 極 17 原 料 氣 體 導 入 開 □ 部 18 反 應 生 成 氣 ΜΑ 體 抽 出 開 口部 2 1 第 一 構 件 22 第 二 構 件 23 第 二 構 件 24 反 應 生 成 氣 體 噴 出 部 25 突 出 部 3 0 第 一 波 紋 管 3 1 第 二 波 紋 管 32 第 —' 筒 狀 構 件 3 3 第 二 筒 狀 構 件 34 收 容 部 3 5 直 h 部 36 擴 徑 部 37 邊 緣 部 3 8 凸 緣 部 39 板 材 40 金 屬 製 容 器 4 1 噴 嘴 42 泵 43 冷 卻 裝 置 44 導 管 45 反 應 生 成 氣 體 導 入 開 口部 -23-16 electrode 17 raw material gas introduction opening portion 18 reaction gas generation body extraction opening portion 2 1 first member 22 second member 23 second member 24 reaction generation gas ejection portion 25 projection portion 3 0 first bellows 3 1 second Bellows 32 - 'Cylinder member 3 3 Second tubular member 34 Housing portion 3 5 Straight portion 36 Expanded portion 37 Edge portion 3 8 Flange portion 39 Plate 40 Metal container 4 1 Nozzle 42 Pump 43 Cooling device 44 conduit 45 reaction to generate gas introduction opening -23-