TW320682B - Method and apparatus for regulating a process for the separation of isomers of aromatic hydrocarbons having from 8 to 10 carbon atoms by a monochromatic light signal - Google Patents
Method and apparatus for regulating a process for the separation of isomers of aromatic hydrocarbons having from 8 to 10 carbon atoms by a monochromatic light signal Download PDFInfo
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- TW320682B TW320682B TW83105961A TW83105961A TW320682B TW 320682 B TW320682 B TW 320682B TW 83105961 A TW83105961 A TW 83105961A TW 83105961 A TW83105961 A TW 83105961A TW 320682 B TW320682 B TW 320682B
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Abstract
Description
經濟部中央標隼局員工消費合作社印製 A7 B7 五、發明説明（） — 本發明係W於一種分離具有8至10倨碳原子芳族碳氫化 合物之異構物方法之調節方法及裝置。 對二甲苯自芳族C*»餾份之’分雄傳铳上由结晶方法或包含 棋擬移動床内吸附之程序實施（參照法國專利91/ 11004 之先前技藝）。鄰二甲苯之分離傳铳上則由超分饑所實施 〇 對於該等方法》欲達成之目的為以鼸著時間仍保持恆定 之方式*製造具有一定純度之異構物。 過低水準之純度會非常嚴重地降低其商莱價值至無法販 賣之程度*而過高水準之純度則會增加操作成本。 迄今為止，以兩種方式可達成純度之檢驗： 1) 在進入或自單元發出之流體内諸點，測定流速及分析 操作，其方式為可對有翮物料建立詳细平衡表，然後，藉 與典型物料平衡表作比較及藉提供各操作變數影響之相闞 性，可對一種或多種操作赛數作修正•以使產率及純度之 值保持在所欲範圍內。建立該種平衡表之頻率每日為1次 至若干次。此意指，不管操作變數上之微小任意變動*為 了確保預定水準之鈍度必須將鈍度之程度訂在稍高目禰上 ，而這對操作成本有不利影響。 2) 利用蒸氣相色雇分析作流出物之線内分析。該法對突 然發生之纯度下降可迅速反應；規格外之產品例如可再循 環，俾不致污染正在填充中之儲定榷*号外•操作變數及 參数之測定可迅速修正通當的設定值。該修正可利用實驗 相W性或利用單元之動態棋擬之软體（其乃基於單元之預 本纸張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） ^ ： ( * 裝 J 务 (請先閏请背面之注意事項再填寫本頁) 32068| 第33105 9 6丨號專利申請案 文說明書修正頁（86年5月） A7 B7 Λ 五、發明説明（） 測性模擬）而實施。”診斷方法問題”一文於Chea. Eng. Prog. V87, No 9, 70-74頁U991)概述最先進的技術狀 況。 關於更精確的對二甲笨純度水準之分析，其可藉氣相色 層分析或測量结晶點而測定。涉及结晶點測定之方法只能 用相當濃（至少8%)的對二甲苯混合物實施，因此其並不 普遍，即使對二甲苯亦然。其亦藉近紅外線光譜學分析 (Ed Stark et col. SPIE Vol 1575，70-86 頁，1991” 可用於近紅外線之光學纖維具有較用於可見光範圍者更高 的衰減係數而不容許使用極大的透射距離。 利用蒸氣相色層分析之分析頻率每小時只能進行很少的 測定，在取樣搡作後僅約十分鐘即產生结果。 然而*在再结晶之情況，設若欲處理之進料的姐成確寅 恆定，則在方法中不同點之精確溫度測定容許對所產生的 對二甲茉純度作極儍異的調節。 然而，在模擬移動床内色層分析之情況*僅測定一參數 如潙度並不會建立純度調節鐽。 經濟部中央標準局貝工消費合作社印製 (請先閲讀背面之注意事項存填寫本貰) 在蒸餾之情況（藉超分餾製造鄰二甲苯），僅測定溫度則 不夠精確，因為300涸實板之全部溫度差異或變異為5至 7Ή。因此，申請人提議同時在多數點（其澍流體相混合 物組成之分離方法為内部）處作即時测量，而測定装置與 分離單元隔開配置。所選之分析方法為拉曼光譜學。 翮於拉曼光譜學於工業環境中溶液之線内即時及多點分 析上之潛動，文獻極多。S M Angel et col. (SPIE Vol 本紙張尺度適用中國國家橾準（CNS ) A4規格（210X297公釐） 經濟部中央標率局員工消費合作社印製 第83105961號專利申請案 r- …！ > .·： —X « 中文說明書修正百（86年5月）A7〃 .d ^ ___Ά 一一_ 五、發明説明（） 1435，超敏感偵檢及分析之光學方法、技術及應用 Π991))說明一種由雷射二極管、PT_拉曼光譜計及CCD 偵檢器（電荷偶合的二極管）所構成之糸統。纖維長度-為 4 m 。為了減弱收集纖維之拉曼光譜，提議二種射出及收 集顯維的組態。纖維之端部彼此以36〇C或l8〇C配置。分 析之溶液為萘及甲苯之純溶液。不用實施定量分析。相同 作者於SPIE Vo丨1587*化學、生化及環境鑛維感應器 III (1991)中，使用相同姐合件以四個雷射二極管供四個 點之同時分析。射出及收集纖维以面向關係定位或形成 15。之角度。收集時間自1至30秒不等。姐合件係用來監 視蒸餾之管柱。在藉蒸餾作水/乙醇分離之情況，乙醇之 百分比係在校正後测定。有關石油餾份蒸餾之潛在應用係 Μ甲笼與苯之百分比之定量化及搜索時間為60秒討論之。 M J Robert et col.於製程控制與品質，1 (1991), 281-291’ Elsevier Science Publishers B.V.阿姆斯特 丹，說明拉曼光譜學，為了化學分析，在線內即時及多點 分析上之限制。其中討論了不同因素如姐份之類型、其數 量、其療度、分析點之數目、精確度之水準及回應時間。 為了免除收集纖維之拉曼光譜，將介質之折射率及纖維相 對於使用波長之衰減考鹿:在内作計算，來決定收集纖維與 射出墦维間之角度。環己烷之拉曼光譜係以35 氧化矽 光學绡維，定位於〗〇〇之角度圼現。 相同作者於 ISA， 1990. 0065-2814/90/463-468 頁，將 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） ----------1------1T------ - 一 *-(請先閲讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消費合作社印製 A7 B7 五'發明説明（） — 下面姐合件應用於水-異丙酵蒸餾管柱之搡作：光滙由 Ya g-Nd雷射所彤成·而櫬械多路調節器可交替地選擇六 個射出纖維之一。射出及接收纖維係由400 m直徑之摻雑 氧化砂氧化_之纖維所構成。光學感應器真正的意義係由 終端有Μ寶石窗之不绣綱管之姐合件所形成，該窗1)在中 心位置有射出纖維，2)在周圍位置有4至6俚收集纖維》 測量室係由90 a· X 50 mm直徑之最小尺寸之圓柱形室所 形成，設有流量計及熱電偁。光譜計設有通濾系統，容許 除去各光譜之Rayleigh擴散信號•收集時間為2.2分鐘· 化學分析之精確度對範圍為5% -95%至95% -5%之混合物 為 3 96 〇 M A Leugers等人於SPFE, Vol 1990，纖維之化學、生 化及環境應用（1988)中，研發一種由中心為收集纖維與其 周圍為6倨接收镰維所形成之探針。此探針用於笨/甲苯 混合物之定量分析。當應用於石油領域時，拉曼光譜學係 用於（美國専利5 139 334)持性之測定*如辛烷數，芳烴 之百分比及單/二芳烴之分佈。美國專利2 527 121討输 了Μ拉曼光譜學澜定烴混合物內之全部芳烴量。 因此，一方面發現全純或經溶劑（4或5俚姐份Κ任何比 例之混合物）稀釋之芳族餵份％之分析從未由該型姐合件 實施，另一方面•混合物甚至二元混合物之定量化仍相當 不精確，且通常不會涵蓋姐成之整：Μ範驛。另一方面，在 先前技藝姐合件中•作者借助於眾多個雷射光源或機械多 路轉換：此等為複雜又昂貴的结構。闞於使用眾多倨光源 本纸張尺度適用中國國家標準（CNS ) Α4規格（210Χ 297公釐） ； ; (‘裝 訂 ^ 务 (請先閱讀背面之注意事項再填寫本页) A7 B7 S20682 五、發明説明（） — •當其為雷射二極管時，光諶寬度通常相當寬而無法獲得 迪於提供具有四或五俚姐份之混合物精確定量化之光譜。 當涉及雷射時，除了成本大增以外，很難提供所有光源精 確地射在相同波長上，此由所得各光譜相互略為移位顯示 出，且無法使用單一定量化软體。另外，所提光學感寧器 及測量室亦昂貴又複雜。最後•在已使用光學孀維之情況 下，其長度從未超出50 使得雷射光源及光饍計完全可 移至控制室或實驗室。然而，以該方式將雷射光源及光譜 計移走為絕對重要，因為企画將複雜又非防爆燃性光學儀 器直接放入工業用分離單元內是不切實際的。 本發明之一目的為規正先前技《之缺點。 另一目的為在分離遇程中在至少一分離區内澜定興構物 混合物内所含至少二種異構物之濃度之分佈情形。 又一目的涉及一種在含有至少二種異構物之混合物中分 離至少一種具有8至10個碳原子芳族碳氫化合物之異構物 方法之調節方法。 又一目的涉及一種於多少稀釋於溶劑如甲苯或對二乙笨 内之芳族C8碳氩化合物混合物中分離對二甲笨方法之調節 方法。 本發明一般係闞於一種分雄至少一具有8至10俚碳原子 芳族破氢化合物之異構物（其包含於一含有至少二種異構 物之混合物内）方法之調節方法C該方孕包含在分離區内 逋當條件下之分離步驟，該法之特徵為： a)波長為400與1300«微米之間’較佳為420與650奄微 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公变） .一，.裝 訂 j線 (請先閏讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消費合作社印製 經濟部中央標準局員工消費合作社印裝 A7 、_ B7 ___ 五、發明説明（） — 米之間之單色光信號同時送至該區之至少二僑逋當點•而 非流出物離開之點， b) 擴散多色光信號係在實質上該點之處回收*對應於 400與3500 cur1之間，較佳600與1200 cb-1之間之拉 曼效應， c) 回收之二信號同時送至一輸送對應拉曼光譜之多槽光 譜計， d) 在該二點每一黏之混合物之化學姐成係自二光譜测定 e) 重複a，b，c及d之顒序，俾可重姐有W包含於混合物 內二異構物濃度之分.佈团•及 f) 所得有鼷濃度之分佈圖與參考濃度分佈圓比較*並對 分離方法之至少一搡作變數採取動作以調節方法。 分析操作之頻率可高達每秒測定一次•而測量與结果間 之延埋可低於100奄秒。因此•對各拥量黏，可得一有關 視時間而定之姐成之曲線，其賁質上為連績性，具有極短 的回應延遲。 依照本發明之諝節方法可以同向流動或逆向流動方式應 用於横擬移動床内吸附方法•而對位之異構物可K稱為萃 取物之皤分，或稱為萃餘物之皤分收集。在該情況•由所 得之濃度分佈圖可調整至少下列搡作變數之一Μ調節方法 * 、 , -溶劑之流速， -進料之流速· 本纸張尺度適用中國國家標準（CNS ) Α4規格（210Χ297公釐） ---：---^---一：裝------訂-----j 線 (請先閏讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消f合作社印製 A7 B7__ 五、發明説明（） — -萃取物以及萃餘物之流速， -所尋求異構物之内回流流速•及 -各吸附程序之毎一區之内流速。 本發明方法亦可應用於至少一俚结晶區内包含對二甲笨 之混合物之结晶方法，且其中，混合物之化學姐成在該區 内至少二不同點測定。在該情況•根據所得濃度分佈_， 可調整至少一下列操作變數Μ調節方法： -溫度 -再洗速率•及 -播拌之速度。 本發明方法亦可使.用於該化合物之混合物之蒸餾》其中 化學姐成係在蒸餾單元內至少二個點，較佳為四倨點測定 。在該情況，根據所得溻縮分佈圓，可調整至少一下列搡 作變數Κ調節方法： -加料之流速 -回流速率 -餾出液之流速 -供應至再沸器之熱量。 本發明之一特微包含通常Κ液相或汽相並在潢度為-70 與+2201C下滴定澴合物之化學姐成。 根據本發明之另一特徵*單色射出信號亦可自所述分離 方法達到至少一流出物，在該情沉下* $化學姐成係根據 本發明之方法測定•流出物之姐成並與參考姐成比較，且 可對方法之搡作變數採取行動。以該方式監視流出物之姐 -10 - 本紙張尺度適用中國國家標準（CNS ) A4現格（210X297公釐） ^ ；~'·裝 訂 Ν 各， 一 (請先閏讀背面之注意事項再填寫本頁) 經濟部中央標孪局負工消費合作社印製 ^20652 A7 、_ B7__ 五、發明説明（） — 成可防止儲存槽被突然降解之產物所污染。本發明可應用 於包含對二甲笨、鄰二甲笨、間二甲笨及乙苯並有溶劑如 甲笨或對二乙苯存在之混合物之分鐮。其亦可應用於包含 芳族％及/或c1〇異構物之混合物之分離。 本發明亦瞄於實施本方法之裝置。 更明確而言·該裝置K姐合方式包含： -單色光信號之雷射或雷射二極管光源，其在可見光範 圍或近紅外線射出，且其接至光束分離器， -至少二光學射出纖維•較佳為至少四俚光學雄維接至 光束分離器， -至少二倨感應器·較佳為至少四個感應器接至光學射 出纖維並配置在分離封閉II之内、外部上·二俚應應器各 配置在封閉«之逋當點*使分析之混合物樣品實質上為均 勻液通， -至少二個光學收集纖維·較佳為至少四個接至感應器 * -至少一多槽拉曼光譜計接至光學收集纖維並逋於產生 代表混合物之拉曼光譜，及 -處理光譜之構件*其接至光譜計並通於連績測定混合 物之化學姐成及有闞混合物濃度之分佈Η。 因此*藉連接至實質上單色光信號之單一光源之光束分 雄器，可在分離封閉體內不同内^提供嚴格相同波長之發 射，藉Κ產生拉曼光譜，其中線之寬度小至可容許定量測 量。 -11 - 本纸張尺度適用中國國家標準（CN'S ) Α4規格（210X297公釐） ^ ； ( ·裝 .1 J 务 (請先閲讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消费合作社印製 A7 、 — —- B7_ 五、發明説明（） 一 根據裝置之一特激，其可包含調節搡作變數之檐件（例 如流虽控制閥），其係由處理構件所控制。更明確而言* 處理構件通常接至電臞，其將所得结果與車先記錄之濃度 分佈圈作比較•且«例如對至少一上述流量調節閥作動· 矯正連鑛記錄的澹度分佈画之傾移或變異。 根據裝置之另一形式•分離封閉體可包合至少二俚光學 殻罩（混合物循環於其中）且其配置在測霣點之位置，且其 各包含一孔口 •較佳由藍寶石製成，面向感應器•各感應 器配置在離孔口最多500 nm之拒離，較佳為50與200 β·之 間。 根據裝置之另一形式•分離封閉體可包含至少二毅箪* (混合物循瓌於其中）且其窗置在測量點之位置，各般罩由 光學射出纖維及收集纖維所穿透，該纗維Μ逋當角度配置 於般罩内，角度係依照混合物之折射率及嫌維之數值孔徑 而計算。 關於工業場所上安全性之需求•該等光學嫌維可具有可 達到1000 η，例如在40與1000 β之間之長度。 長度為50至400 之纖維可得良好结果。 本發明由下列《示本發明方法及装罝之附圓當可更加明 白，其中： Η1顯示本發明之装置， 圖2顯示依照波數而定之具有^價碳原子之芳族異構物 之混合物之拉曼信號光學強度*及 _ 画3至7顯示供對二甲苯分難用之具有8儷碳原子芳族 -12 - 本紙張適用中國國家標孪（CNS ) Α4現格（210Χ297公釐） ^ .. ( 裝 訂 . γ 威 (讀先閱讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消f合作社印袈 A7 、_ B7___ 五、發明説明（） — 碳氫化合物混合物之不同異構物之禳度之分佈圓。 概示於圓1之裝置分成二俚區域，一俚區域有雷射光源 1及拉曼光譜計6 ，另一區域為一供芳族“異構物分離之 装置9 (例如模擬逆流移動床）*其上S置有感應器4 。二 區域由八根纖維3，5所連接：四根纖維3傳送雷射之激發 光至感應器4 ，而另四根纖維5則將感應器之擴散信號回 送至光譜計6 。 自雷射發出時，光束集中在商業上可得之光束分雕器2 之入口嫌維上（參照SEDI偶合器卜4)，其同時將單色激發 信號送至吸附管柱9內之代表性樣品。另一姐合件（匾中 未示）涉及將光束送至光學多路調節器（分離装置之網路 或格柵）並將四光束集中在四根嫌維3上。 姐合件所用之光學嫌維為氧化矽，具有核心為lOOw·及 全部直徑為125 (數值孔徑為0.22)。感應器4有二型· 端視溫度低於或高於801C而定。在80t：以下，感應器 ” Super Dilor Head”M回散射形式在光學殼罩8孔口 7之 外側上操作，殻罩係安裝在吸附管柱9上且混合物循環於 其中。纖雄直接接至感應器。須知，其可热涵緣”Super Dilor Head"，其方式為，其溫度保持在80XJK下，而在 孔口後流動之分析混合物則在較高溫度下。在80ΌΜ上， 於另一具體例中，接至感應器4a之射出鐡維3 a及收集纖維 5a，彼此相互Μ 15。之角度穿入采學殻罩8a内並直接放入 涓合物中。密封整通性係藉塞填盒子（圖中未示）確保。須 知，高溫（高達280 Ό)必須使用特殊纖維。” Super -13 - 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） ^ „ 一 裝 訂务 (請先閏讀背面之注意事項再填寫本頁) 經濟部中央標孪局員工消费合作社印裝 Μ > — " _Β7_ 五、發明説明（） 一Printed by the Employee Consumer Cooperative of the Central Standard Falcon Bureau of the Ministry of Economic Affairs. A7 B7 V. Description of the invention () — The present invention is a method and device for adjusting a method for separating isomers of aromatic hydrocarbons having 8 to 10 carbon atoms. Para-xylene is carried out from the aromatic C * »fraction ’s‘ breast ’by the crystallization method or the procedure involving adsorption in a moving bed (refer to the prior art of French Patent 91/11004). The separation and transfer of o-xylene is carried out by super-digestion. For these methods, the aim is to produce isomers with a certain degree of purity in a way that keeps the elapsed time constant. Too low a level of purity will severely reduce its merchant value to the point where it cannot be sold * and too high a level of purity will increase operating costs. So far, the purity test can be achieved in two ways: 1) at various points in the fluid entering or coming from the unit, the flow rate and the analysis operation are measured, in such a way that a detailed balance table can be established for the material with 翮, and then, by Comparing with the typical material balance table and providing the phase difference of the influence of each operation variable, one or more operation race numbers can be modified to keep the yield and purity values within the desired range. The frequency of establishing this balance sheet is from 1 to several times a day. This means that, regardless of small arbitrary changes in operating variables *, in order to ensure a predetermined level of bluntness, the degree of bluntness must be set at a slightly higher level, which has an adverse effect on operating costs. 2) Use vapor phase color analysis for in-line analysis of effluent. This method can react quickly to the sudden decrease in purity; products outside the specifications can be recycled, for example, so as not to contaminate the storage tanks that are being filled. The measurement of operating variables and parameters can quickly correct the appropriate set values. The correction can use experimental compatibility or dynamic software using the unit (which is based on the paper format of the unit's pre-preparation. It is applicable to the Chinese National Standard (CNS) A4 specification (210X297mm) ^: (* Install J service ( Please fill in the notes on the back before filling in this page) 32068 | No. 33105 9 6 丨 Patent application text specification revision page (May 86) A7 B7 Λ 5. Invention description () Test simulation) to implement. " "Diagnostic method problems" in Chea. Eng. Prog. V87, No 9, pages 70-74 (U991) outlines the state of the art. For more accurate analysis of the purity level of dimethylbenzidine, it can be determined by gas chromatography or measurement of the crystallization point. The method involving the determination of the crystallization point can only be carried out with a very concentrated (at least 8%) mixture of para-xylene, so it is not universal, even para-xylene. It also uses near-infrared spectroscopy (Ed Stark et col. SPIE Vol 1575, pages 70-86, 1991 ”. Optical fibers that can be used in near-infrared have a higher attenuation coefficient than those used in the visible range and do not allow the use of extremely large Transmission distance. The analysis frequency using vapor phase chromatography can only make few measurements per hour, and the result will be produced only about ten minutes after sampling. However, in the case of recrystallization, suppose that the feed is to be processed The sister temperature is constant, the precise temperature measurement at different points in the method allows extremely silly adjustments to the purity of the produced dimethanone. However, in the case of chromatographic analysis in a simulated moving bed * only one parameter is measured For example, the degree of purity will not be established. Printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back and fill in this file). In the case of distillation (manufacturing o-xylene by super-fractionation) The measurement of temperature is not accurate enough, because the overall temperature difference or variation of the 300-solid board is 5 to 7Ή. Therefore, the applicant proposes to simultaneously at most points (the composition of the fluid phase mixture is The measurement method is internal), and the measurement device is separated from the separation unit. The selected analysis method is Raman spectroscopy. The real-time and multi-point analysis in the line of the solution in the industrial environment. There is a lot of literature on it. SM Angel et col. (SPIE Vol) This paper standard is applicable to China National Standard (CNS) A4 (210X297mm) Patent No. 83105961 printed by the Employees Consumer Cooperative of the Central Bureau of Standards and Statistics of the Ministry of Economic Affairs Application case r-…! ≫. ·: —X «Chinese manual revision 100 (May 86) A7〃 .d ^ ___ Ά 一一 _ V. Invention description () 1435, optical method for ultra-sensitive detection and analysis , Technology and application Π991)) Describe a system consisting of laser diode, PT_Raman spectrometer and CCD detector (charge coupled diode). Fiber length-4 m. In order to weaken the pull of the collection fiber Mann Spectroscopy proposes two configurations for projecting and collecting apparent dimensions. The ends of the fibers are arranged at 36 ° C or 18 ° C. The solution analyzed is a pure solution of naphthalene and toluene. No quantitative analysis is required. The same author is at SPIE Vo 丨 1587 * Chem In the chemical, biochemical, and environmental mine dimension sensor III (1991), four laser diodes are used for the simultaneous analysis of four points using the same sister piece. The fibers are emitted and collected to position the relationship or form an angle of 15. The collection time varies from 1 to 30 seconds. The sister piece is used to monitor the column of distillation. In the case of distillation for water / ethanol separation, the percentage of ethanol is determined after calibration. Potential applications for petroleum fraction distillation The quantification of the percentage of M cage and benzene is discussed and the search time is 60 seconds. MJ Robert et col. In Process Control and Quality, 1 (1991), 281-291 'Elsevier Science Publishers BV Amsterdam, illustrating Raman spectroscopy For the purpose of chemical analysis, there are limitations on real-time and multi-point analysis in the line. It discusses different factors such as the type of sister serving, its number, its treatment, the number of analysis points, the level of accuracy and response time. In order to avoid the Raman spectrum of the collected fiber, the refractive index of the medium and the attenuation of the fiber relative to the wavelength used are considered: to calculate the angle between the collected fiber and the emission dimension. The Raman spectrum of cyclohexane is based on the 35 silica optical dimension, which is located at an angle of 〖〇〇. The same author on ISA, 1990. 0065-2814 / 90 / 463-468 pages, the paper size is applicable to the Chinese National Standard (CNS) A4 specification (210X 297 mm) ---------- 1-- ---- 1T -------1 *-(please read the notes on the back before filling in this page) A7 B7 5 'invention description printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs () — The following sister The piece is used in the operation of water-isopropyl fermentation distillation column: the light sink is formed by the Ya g-Nd laser. The mechanical multi-way regulator can alternately select one of the six injection fibers. The injection and receiving fibers are composed of 400 m diameter oxidized sand-doped fibers. The true meaning of the optical sensor is formed by the sister assembly of the non-stitched tube with a M gem window at the end. The window 1) has an ejected fiber at the center position, 2) 4 to 6 squaring fibers are collected at the surrounding position. The chamber is formed by a cylindrical chamber with a minimum size of 90 a · X 50 mm in diameter, equipped with a flow meter and a thermoelectric cell. The spectrometer is equipped with a pass filter system that allows the removal of the Rayleigh diffusion signals of each spectrum. • The collection time is 2.2 minutes. • The accuracy of chemical analysis is 3 96 〇MA Leugers for mixtures ranging from 5% -95% to 95% -5%. In SPFE, Vol 1990, Fiber, Chemistry, Biochemistry, and Environmental Applications (1988), we developed a probe formed by the center for collecting fibers and the surrounding 6-bit receiving Siwei. This probe is used for quantitative analysis of Ben / toluene mixtures. When applied to the petroleum field, the Raman spectroscopy system is used to determine the persistence of (US 5139139) * such as the number of octanes, the percentage of aromatic hydrocarbons, and the distribution of mono / diaromatic hydrocarbons. U.S. Patent No. 2,527,121 discusses the total amount of aromatic hydrocarbons in the M Raman spectroscopy Landing hydrocarbon mixture. Therefore, on the one hand, it was found that the analysis of% pure aromatic or diluted with solvent (mixture of 4 or 5 Mie parts K in any proportion) has never been carried out by this type of sister, on the other hand • the mixture is even binary The quantification of the mixture is still quite inaccurate, and usually does not cover the whole sister: M Fanyi. On the other hand, in the previous art piece, the author resorted to numerous laser light sources or mechanical multiplexing: these are complex and expensive structures. Kan is using many light sources. The paper standard is applicable to the Chinese National Standard (CNS) Α4 specification (210Χ 297 mm);; ('Binding ^ service (please read the precautions on the back and fill in this page) A7 B7 S20682 V. Description of the invention ()-• When it is a laser diode, the photon width is usually quite wide and it is impossible to obtain a spectrum that provides accurate quantification of a mixture with four or five parts. When it comes to laser, except for the large cost In addition, it is difficult to provide that all light sources are accurately shining on the same wavelength, which is shown by the slight shift of each spectrum obtained, and it is impossible to use a single quantitative software. In addition, the optical sensor and measurement room mentioned are also expensive and Complicated. Finally, in the case where optical widows have been used, its length never exceeds 50 so that the laser light source and light meal meter can be completely moved to the control room or laboratory. However, in this way, the laser light source and spectrometer Removal is absolutely important because it is impractical to plan to put complex and non-explosion-proof optical instruments directly into industrial separation units. One of the purposes of the present invention is to regulate the previous "The shortcomings. Another purpose is to determine the distribution of the concentration of at least two isomers contained in the mixture of Landingxing structures in at least one separation zone during the separation process. Another object relates to a solution containing at least two kinds of isomers. A method for regulating the separation of at least one isomer of aromatic hydrocarbons having 8 to 10 carbon atoms from a mixture of isomers. Another object relates to an aromatic compound diluted in a solvent such as toluene or p-diethylbenzene Group C8 carbon argon compound mixture separation method for the regulation of the dimethyl stupid method. The present invention is generally based on an isomer of at least one aromatic hydrogen-breaking compound having at least 8 to 10 carbon atoms (which is contained in a Within a mixture of at least two isomers) Method of adjustment method C. This method includes a separation step under the prevailing conditions in the separation zone. The characteristics of this method are: a) The wavelength is between 400 and 1300 microns Jiawei's 420 and 650 micro-sheet paper standards are applicable to the Chinese National Standard (CNS) A4 specification (210X297 commutation). 1. Binding j line (please read the notes on the back before filling this page) Member of the Central Standards Bureau of the Ministry of Economy Industrial and consumer cooperatives print A7, _B7 ___ printed by employees ’consumer cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of invention () — Monochromatic light signals between meters are sent to at least two overseas Chinese at the same time The point where the effluent leaves, b) The diffuse polychromatic light signal is recovered at that point essentially * corresponds to the Raman effect between 400 and 3500 cur1, preferably between 600 and 1200 cb-1, c) recovered The two signals are sent to a multi-slot spectrometer corresponding to the Raman spectrum at the same time. D) The chemical composition of each viscous mixture at the two points is measured from the two spectra. E) Repeat the sequence of a, b, c and d. , Bi Kezhong has the concentration of the two isomers contained in the mixture. Cloth • and f) The obtained distribution map of the concentration of the compound is compared with the reference concentration distribution circle * and at least one of the separation methods is used as a variable Action to adjust the method. The frequency of analysis operations can be measured up to once per second. • The embedding between measurement and results can be less than 100 msec. Therefore, sticking to each volume, you can get a curve that depends on the time, which is continuous in nature and has a very short response delay. The method according to the present invention can be applied to the adsorption method in a horizontally moving bed in a co-current or counter-flow mode. The para-isomer can be called the extract of the extract, or the extract of the raffinate. Sub-collection. In this case • From the obtained concentration profile, at least one of the following operation variables can be adjusted. Μ Adjustment method *,, -The flow rate of the solvent, -The flow rate of the feed material · This paper scale is applicable to the Chinese National Standard (CNS) A4 specifications ( 210Χ297mm) ---: --- ^ --- One: Install ------ order ----- j line (please read the notes on the back before filling this page) Ministry of Economic Affairs Central Standards A7 B7__ printed by the bureau employees' cooperatives V. Description of the invention ()--the flow rate of the extract and the raffinate,-the reflux flow rate within the isomer sought • and-the flow rate within each zone of each adsorption process. The method of the present invention can also be applied to the crystallization method of a mixture containing p-dimethyben in at least one crystallization zone, and wherein the chemical composition of the mixture is determined at at least two different points in the zone. In this case • according to the obtained concentration distribution, at least one of the following operating variables M adjustment method can be adjusted:-temperature-rewash rate • and-sowing speed. The method of the present invention can also be used for the distillation of a mixture of the compounds, wherein the chemical components are measured in at least two points, preferably four points, in the distillation unit. In this case, according to the obtained constriction distribution circle, at least one of the following adjustment methods for variable K can be adjusted:-the flow rate of the feed-the reflux rate-the flow rate of the distillate-the amount of heat supplied to the reboiler. One of the features of the present invention includes the chemical composition of the usual K liquid phase or vapor phase and titration of the complex at a temperature of -70 and + 2201C. According to another feature of the present invention * The monochromatic injection signal can also achieve at least first-class output from the separation method, and sinks in this situation * $ Chemical sister is determined according to the method of the present invention Refer to the sister comparison, and take action on the method's variables. Sister -10 for monitoring the effluent in this way-This paper scale is applicable to the Chinese National Standard (CNS) A4 cash (210X297 mm) ^; ~ '· Binding Ν each, one (please read the notes on the back before filling in This page) Printed by the Consumer Labor Cooperative of the Central Standardization Bureau of the Ministry of Economic Affairs ^ 20652 A7, _B7__ 5. Description of the invention () — It can prevent the storage tank from being contaminated by the products of sudden degradation. The present invention can be applied to a split containing a mixture of p-dimethylbenzyl, o-dimethylbenzyl, m-dimethylbenzyl, and ethylbenzene in combination with a solvent such as methylbenzyl or p-diethylbenzene. It can also be applied to the separation of mixtures containing aromatic% and / or C10 isomers. The invention also aims at the device for implementing the method. More specifically, the K-joint method of the device includes:-Monochromatic light signal laser or laser diode light source, which is emitted in the visible range or near infrared, and it is connected to the beam splitter,-at least two optical exit fibers • It is preferred that at least four optical fibers are connected to the beam splitter,-at least two sensors. Preferably, at least four sensors are connected to the optical exit fiber and are arranged inside and outside the separation enclosure II. The applicator should be arranged at the closed point of «to make the analyzed sample of the mixture substantially liquid-passing,-at least two optical collection fibers, preferably at least four connected to the sensor *-at least one multi-slot pull The Mann spectrometer is connected to the optical collection fiber and used to generate a Raman spectrum representing the mixture, and-a component to process the spectrum . Therefore, by means of a beam splitter connected to a single light source of substantially monochromatic light signal, it can provide strictly the same wavelength emission in different interiors of the separation enclosure, and generate a Raman spectrum by K. The width of the line is as small as acceptable Quantitative measurement. -11-This paper scale is applicable to the Chinese National Standard (CN'S) Α4 specification (210X297mm) ^; (· Packing. 1 J task (please read the precautions on the back before filling this page) Employee consumption of the Central Standards Bureau of the Ministry of Economic Affairs A7 printed by the cooperative, — —- B7_ V. Description of the invention (1) According to one of the devices, it can contain eaves (such as flow control valves) that are adjusted as variables, which are controlled by the processing components. Specifically, the processing component is usually connected to the electro-hydraulic, which compares the obtained result with the concentration distribution circle recorded by the vehicle first • and «e.g. actuates at least one of the above-mentioned flow regulating valves According to another form of the device, the separation enclosure can enclose at least two optical covers (the mixture circulates in it) and it is arranged at the position of the measuring point, and each of them contains an orifice. Made of sapphire, facing the sensor • Each sensor is placed at a rejection of up to 500 nm from the orifice, preferably between 50 and 200 β ·. According to another form of the device • The separation enclosure may contain at least two yi ji * (Mixed Follow it) and its window is located at the measuring point, each cover is penetrated by the optical exit fiber and the collection fiber, the angle of the dimension is arranged in the cover, the angle is based on the refractive index of the mixture and the The numerical aperture of the dimension is calculated. Regarding the need for safety in industrial sites • These optical dimensions can have a length of up to 1000 η, for example between 40 and 1000 β. Fibers with a length of 50 to 400 can give good results The present invention can be more clearly understood from the following "The attached circle showing the method and the decoration of the present invention, in which: Η1 shows the device of the present invention, and FIG. 2 shows the aromatic isomers with valent carbon atoms depending on the wave number. The optical intensity of the Raman signal of the mixture * and _ Drawings 3 to 7 show the aromatic-12 with 8 litre carbon atoms for p-xylene separation-This paper is suitable for China National Standard (CNS) Α4 present grid (210Χ297mm ) ^ .. (Binding. Γ Wei (read the precautions on the back before filling in this page) Employee Consumers of the Central Bureau of Standards of the Ministry of Economic Affairs Co-op A7, _ B7___ V. Description of invention () — Difference of hydrocarbon mixture Heterogeneous The distribution of the degree of the circle. The device outlined in circle 1 is divided into two singular regions, one singular region has a laser light source 1 and a Raman spectrometer 6, the other region is a device for the separation of aromatic “isomers 9 (For example, to simulate a counter-current moving bed) * S is placed on the sensor 4. The two areas are connected by eight fibers 3, 5: four fibers 3 transmit the laser excitation light to the sensor 4, and the other four fibers 5 The diffuse signal of the sensor is sent back to the spectrometer 6. When the laser is emitted, the beam is concentrated on the entrance dimension of the commercially available beam splitter 2 (refer to SEDI coupler 4), which will The color excitation signal is sent to the representative sample in the adsorption column 9. Another sister piece (not shown in the plaque) involves sending the beam to the optical multiplexer (separating device network or grid) and concentrating the four beams on the four dimensions 3. The optical dimension used by the sister assembly is silicon oxide, with a core of 100w · and an overall diameter of 125 (numerical aperture is 0.22). The sensor 4 has two types. The end depends on the temperature below or above 801C. At 80t: below, the sensor "Super Dilor Head" M backscattering mode is operated on the outside of the orifice 7 of the optical enclosure 8, the enclosure is mounted on the adsorption column 9 and the mixture circulates in it. Slender male is directly connected to the sensor. It should be noted that its thermal boundary "Super Dilor Head" is maintained in such a way that its temperature is maintained at 80XJK, and the analytical mixture flowing behind the orifice is at a higher temperature. At 80ΌΜ, in another specific example , The ejection dimension 3a and the collection fiber 5a which are connected to the sensor 4a, penetrate each other at an angle of 15 ° into the mining enclosure 8a and directly into the trickle. The sealing integrity is to fill the box by plugging (Not shown in the picture) Make sure. Note that special fibers must be used at high temperatures (up to 280 Ό). "Super -13-This paper scale is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) ^„ One binding order (please Read the precautions on the back first and then fill out this page) Printed by the Consumer Cooperative of the Central Standardization Bureau of the Ministry of Economic Affairs Μ > — " _Β7_ V. Description of invention () 1
Di Ur Head"為已知裝置，其用來防止激發光進入回轉嫌 維中並在其内產生氧化矽之拉曼光譜。侵入糸統具有相同 特微，至少是藺於涉及芳族Ce分子之分離方法之分子•但 其發光較低。然而，其可抗拒髙溫，不像"Super Dilor Head" ° 光學妓罩為相同類型並藉遘當接頭安装在單元之導管上 。對於"Super Dilor Head”*其設有藍寶石之孔口。在二 根纖維進入光學般罩之情況，藍寶石由板所取代•其中安 装有钃維之塞填盒子。所有纖維接頭為檷準犁（SNA 905) •包括對光譜計之接頭。 八根纖維可接至拉曼光譜計6之入口。象散糸统10可同 時獲得八個對應光譜，在（TCD(«荷偶合二極管）偵檢器 (2次元多槽）上成移位闞係，且藉重複相同步驟之順序， 利用逋當電臞在分離管柱内可得有Μ混合物姐份濃度之分 佈画。另外，數據處理構件可控制一闕而控制萃取物如 11所示之流速*或一泵而控制溶劑如12所示之流速。 對二甲苯分離過程所遣遇之分子之拉曼光譜在槿廣大光 譜範圍（0至3,500 c·-1)内具有略為明顯線條。但锊要發 現一充分減少至使其同時可由偵檢器看見之範園，且其中 欲分析之每一姐份有一至少充分微细而明顯之線•較佳範 圃為67 5至915 cur1。Η2所示之光譜顯示該範圍之灌部 (其無任何發射）可測定基線*式各分子都有一線。 有闞濃度之計算係藉測定尖峰之高_度而進行。矩陣計算 可考慮重疊。設I為分子所得線之明度，並設Mj為實測 -14 - 本纸張尺度適用中國國家樣準（CNS ) A4規格（210X297公釐） ! ^1 J { 裝"~ HII I 1-·線 (請先閏讀背面之注意事項再填寫本頁) 經濟部中央標準局負工消f合作社印裝 320682 A7 ^ 一 · B7 五、發明説明（） - 明度。由此得： ΣDi Ur Head " is a known device, which is used to prevent excitation light from entering the rotation dimension and generating a Raman spectrum of silicon oxide therein. The intrusive system has the same features, at least the molecules involved in the separation method involving aromatic Ce molecules • but its luminescence is low. However, it can resist high temperature, unlike " Super Dilor Head " ° The optical brothel is of the same type and is installed on the unit's conduit by a suitable connector. For " Super Dilor Head ”* it is equipped with a sapphire orifice. In the case where two fibers enter the optical cover, the sapphire is replaced by a plate • There is a plug-in box filled with dimensional Wei. All fiber joints are quasi-plow (SNA 905) • Including the connector to the spectrometer. Eight fibers can be connected to the entrance of the Raman spectrometer 6. The astigmatism system 10 can obtain eight corresponding spectra at the same time. The device (multi-dimensional multi-slot) has a shifting system, and by repeating the sequence of the same steps, the distribution map of the concentration of the M mixture in the separation column can be obtained by using the electric shock in the separation column. In addition, the data processing component can be Control a flow rate and control the flow rate of the extract as shown in 11 * or a pump and control the flow rate of the solvent as shown in 12. The Raman spectrum of the molecules encountered in the paraxylene separation process is in the broad spectral range of Hibiscus (0 to 3,500 c · -1) has slightly obvious lines. However, it is necessary to find a fan garden that is sufficiently reduced to be visible to the detector at the same time, and each sister to be analyzed has at least a sufficiently fine and obvious line. Jiafanpu is 67 5 to 915 cur1 The spectrum shown in Η2 shows that the irrigation part of this range (which does not have any emission) can be measured in the baseline * formula. Each molecule has a line. The calculation of the concentration of Kan is performed by measuring the height of the peak. The matrix calculation can consider overlap . Let I be the brightness of the line obtained by the molecule, and let Mj be the actual measurement -14-This paper scale is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm)! ^ 1 J {装 " ~ HII I 1- · Line (please read the precautions on the back before filling in this page) Printed by the Ministry of Economic Affairs, Central Standards Bureau, Cooperative Society 320682 A7 ^ 1 · B7 5. Description of invention ()-Brightness. From this: Σ
Mj = jC i j · Ij (1) 係數cn係基於純產物之光譜而測定。設[k]為係数 Cij之矩陣，設[I]為IJ之矩陣而設[Μ]為Mj之矩陣。由 此得：[I] = [k-1] · [M] (2) 然後，烴相對有效擴散段標準化之明度Ij即與分子之相 對密度成比例。值j係由等冥耳二元混合物之光譜所得。 最後*分子j之濃度由以下表示：Mj = jC i j · Ij (1) The coefficient cn is determined based on the spectrum of the pure product. Let [k] be the matrix of coefficients Cij, let [I] be the matrix of IJ and let [M] be the matrix of Mj. It follows: [I] = [k-1] · [M] (2) Then, the normalized lightness Ij of the hydrocarbon relative to the effective diffusion section is proportional to the relative density of the molecules. The value j is obtained from the spectrum of the binary mixture of equal ears. Finally, the concentration of molecule j is represented by the following:
Cj = Ij/Ω j Σ Ij/Ω j (3) 須知，測定值Qj之操作亦涉及矩陣計算以考Λ可能的 重疊。另外•與湛度有翮之值Cj及值Ω j必須為巳知。 雖然較佳是薄离度方法進行有Μ濃度水準之計算*惟在 線實質擴大之情況（例如在高溫下），可採用表面積之方法 ，巳知各線由羅倫茲（Lorentz)曲線所表示*且在干擾之 情況，為此等曲線之去彎曲箝要進行計算。 下列實例例示本發明： 奮锎1 : 表I說明對五種姐份，對、間、鄰二甲苯、乙苯及甲苯 之各種混合物進行之測定之结果。所示者為實濃度1)及由 拉曼光譜學2)及3)在檐2)上所测运:者，檐直接接至光譜計 宏鎗入及在利用光學纖維3)移位200 j«後。光譜例示於圓 2 *其中混合物5之拉曼信號之光學強度係對波數繪製， -15 - 本紙張尺度適用中國國家榡準（CNS ) A4規格（210X297公釐） | 『 裝 訂 y 务 (請先Μ讀背面之注意事項再填寫本頁) 經濟部中央標隼局員工消費合作社印製 A7 B7_ 五、發明説明（） 一 收集時間為10秒。表I顯示賁際上依照累積测定之數所得 之精確度：可知10秒之期間即已足夠。 在二表中，所用波長為514.5 ，Ml.3 W動力離子化 氬雷射獲得。此等光譜係得自拉曼光譜計，Dilor型XY。 計算套裝軟體係裝設在PC型486上。 音俐2 : 此例使用棋擬移動床實驗分離軍元，由24個長度為1 b 及直徑為1 c·之管柱所姐成*裝填有KBa交換的沸石Y 。 在各管柱之間，可利用四個姐合件（相等於四個24加單向 閥）導入進料或溶劑或者其他Μ取出萃取物或萃餘物。此 項裝置巳述於法國專$ 91/1 1004及一書：製備與生產規棋 之色層分析術，G B a r k e r *a n d G G a n e s t 〇 s M a r c e 1 Dekkar公司，妞約版，1992年9月· 301 -349頁。 與該二引例之說明比較•已加入四俚室，其中液厢流出 且在該處終端係接至實例1光源雷射之200 光源光學鑛 維及接至Μ實例1接收器2D矩陣接至光諝計之200 1«接收 光學嫌維。其分別配置在管柱4與5之間、管柱12與13之 間、管柱20與21之間及多位萃取閥輿萃取物排放泵之間。 所選洗提溶劑為甲苯。 進料之组成如下：甲笨2.276 %、乙笨11.120%、對二 甲笨22.453%、間二甲苯49.708¾、鄰芋甲苯14.351¾。 整個裝置溫度提高至1 50υ。 -16 - 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ297公釐） ^ ^ ( 裝 訂 Υ;線 (锖先閱讀背面之注意事項再填寫本頁) 經濟部中央標準局HIJ工消費合作社印製 A7 B7 五、發明説明（） 表_1:八個混合物之濃度：1)公佈者2)榷內澜定者3)M125 W·纖維 ^者。在後者情況*混合物距光譜計及激發器雷射2〇〇 »。 混合物 濃度 (' 1甲苯 1 丨間二甲苯丨 1 對二甲苯丨 鄰二甲苯 1 丨 乙苯 1公佈者 | 97 1 〇 3 1 0 1 〇 混合物1 2槽内者 | 96,90 1 〇,〇S 2(9B 1 0,06 (),00 1 γ 3纖維者 | 96,的 | 1 -〇π | | 3,00 1 | 0,^4 0肩 1 1 1公佈者 | 82 i 〇 1 1 〇 0JL> 1 1 混合物2 2槽內者 | 82,34 1 〇,〇〇 1 )7,0^ 1 -0.05 0.0] 1 3嫌維者 I 81#05 I 1-0.06 1 1 j 17,92 1 | 0·〕7 0 J ] 1 1公佈者 1 | 82 ! 1 I 0J5 1 ]7,85 I 1 0 〇 1 1 混合物3 2槽内者 | 81,97 1 0J7 1 17,99 1 -0,03 -0 JO I 3纖維者 | 03,53 1 -0,05 1 38.00 1 0,28 0J!3 1 1公佈者 1 | Β2 I 1 1 〇J〇 1 ]7,70 1 1 0，] 5 1 1 混合物4 2槽内者 | 02.^5 1 〇.”）1 r;,no 1 0,02 -0.0? 1 3嫌維者 | 03.85 1-0.08 1 ί t 17,79 1 -0,0] 0,^3 1 1公佈者 1 | 50 1 I 1 3,5 1 25 1 t J ,5 20 1 1 混合物5 2槽内者 | 49,9j i 3,43 I ^ b # ύ ] 1 】.3a 19,76 i 3潘維者 卜 9,〕5 I 3,27 1 2Gr02 1 J ,50 ] 1 1公佈者 1 ! 2 1 1 | 50 1 1 _ 1 1 1 r； 丨 30 i T 混合物6 2槽內者 .1 3.00 | 49,犯 1 -0,93 i ]7,28 1 、30,]。〜 」· 3纖維者 | 2.?0 I ^8,5J . | 1 .06 1 17,53 [ 30.^7 Γ 1公佈者 1 | 30 1 - 1 1 35 0,5 1 1 i 12,5 | 1 混合物7 2槽内者 | 29,36 | 35.-13 | 0,5^ 1 ]2,76 | 1 3嫌維者 | 29,30 1 I .3已.52 1 I 1 0,47 1 1 | 1 P.2.28 I 1 1公佈者 | 65 p.o 1 〇 1 】0 | 5 1 混合物8 2槽内者 | 65,60 J9.79 I -0.0^ 1 D.B9 | 4#95 1 3纖維者 1 〇4, J 9 J 3 1 -0.2B 1 9,55 | 4,9G 1 1 17 - ^ ^ 裝 訂 ^ 泠 (請先閱讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標隼（CNS ) A4規格（210X 297公釐） ^20682 A7 B7 五、發明説明（） —Cj = Ij / Ω j Σ Ij / Ω j (3) It should be noted that the operation of the measured value Qj also involves matrix calculation to account for possible overlap. In addition, the value of Cj and the value of Ω j, which are related to Cham, must be known. Although it is preferable to use the thin ionization method for the calculation of the M concentration level *, however, when the line is substantially expanded (for example, at high temperatures), the surface area method can be used. It is known that each line is represented by the Lorentz curve * and In the case of interference, the calculation of bending pliers for this curve is required. The following examples illustrate the present invention: Fen cal 1: Table I illustrates the results of the determination of five mixtures of various mixtures of p-, m-, o-xylene, ethylbenzene and toluene. Shown are the actual concentration 1) and measured by Raman spectroscopy 2) and 3) on the eaves 2): the eaves are directly connected to the spectrometer macro gun and used optical fiber 3) shift 200 j "Rear. An example of the spectrum is shown in circle 2 * where the optical intensity of the Raman signal of mixture 5 is plotted against the wave number, -15-This paper scale is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) | "Binding y Read the precautions on the back first and then fill out this page) A7 B7_ printed by the Employee Consumer Cooperative of the Central Standard Falcon Bureau of the Ministry of Economic Affairs V. Description of the invention () A collection time is 10 seconds. Table I shows the accuracy based on the cumulatively measured numbers: it can be seen that a period of 10 seconds is sufficient. In the second table, the wavelength used is 514.5, obtained by Ml.3 W power ionization argon laser. These spectra were obtained from Raman spectrometer, Dilor type XY. The computing system soft system is installed on the PC type 486. Yin Li 2: In this example, a quasi-moving bed experiment was used to separate the army. The 24 columns of 1 b in length and 1 c in diameter were filled with KBa-exchanged zeolite Y. Between each column, four sisters (equivalent to four 24 plus one-way valves) can be used to introduce feed or solvent or other M to extract extracts or raffinates. This device is described in the French special $ 91/1 1004 and a book: Preparation and Production of Chromatic Chromatography, GB arker * and GG anest 〇s M arce 1 Dekkar, Niuyue, September 1992 · 301-349 pages. Comparing with the description of the two cited examples • A four-segment chamber has been added, in which the liquid chamber flows out and the terminal is connected to the optical source of the 200 light source of the example 1 light source laser and connected to the M example 1 receiver 2D matrix to the light No. 200 1 «Receive optical suspected dimension. They are arranged between the columns 4 and 5, between the columns 12 and 13, between the columns 20 and 21, and between the multiple extraction valves and the extract discharge pump. The selected elution solvent is toluene. The composition of the feedstock is as follows: methylbenzine 2.276%, ethylbenzine 11.120%, p-dimethylbenzane 22.453%, m-xylene 49.708¾, o-toluene 14.351¾. The temperature of the whole device is increased to 150V. -16-This paper scale is applicable to the Chinese National Standard (CNS) Α4 specification (210Χ297mm) ^ ^ (Binding Υ; line (read the precautions on the back before filling this page) HIJ Industrial and Consumer Cooperatives Central Bureau of Economic Affairs of the Ministry of Economic Affairs System A7 B7 V. Description of the invention () Table_1: Concentration of eight mixtures: 1) Published by 2) Inquired by 3) M125 W · Fiber ^. In the latter case, the mixture is 200 ° away from the spectrometer and the excimer laser. Mixture concentration ('1 toluene 1 丨 m-xylene 丨 1 p-xylene 丨 o-xylene 1 丨 ethylbenzene 1 publisher | 97 1 〇3 1 0 1 〇 mixture 1 2 in the tank | 96,90 1 〇, 〇 S 2 (9B 1 0,06 (), 00 1 γ 3 fiber | 96, of | 1 -〇π | | 3,00 1 | 0, ^ 4 0 shoulder 1 1 1 publisher | 82 i 〇1 1 〇0JL> 1 1 mixture 2 2 in the tank | 82,34 1 〇, 〇〇1) 7,0 ^ 1 -0.05 0.0] 1 3 suspected dimension I 81 # 05 I 1-0.06 1 1 j 17,92 1 | 0 ·] 7 0 J] 1 1 publisher 1 | 82! 1 I 0J5 1] 7,85 I 1 0 〇1 1 mixture 3 2 in the tank | 81,97 1 0J7 1 17,99 1 -0 , 03 -0 JO I 3 fiber | 03,53 1 -0,05 1 38.00 1 0,28 0J! 3 1 1 publisher 1 | Β2 I 1 1 〇J〇1] 7,70 1 1 0,] 5 1 1 mixture 4 2 in the tank | 02. ^ 5 1 〇. ”) 1 r;, no 1 0,02 -0.0? 1 3 suspected dimension holder | 03.85 1-0.08 1 ί t 17,79 1 -0 , 0] 0, ^ 3 1 1Publisher 1 | 50 1 I 1 3,5 1 25 1 t J, 5 20 1 1 Mixture 5 2 Insider | 49,9j i 3,43 I ^ b # ύ] 1】 .3a 19,76 i 3 Pan Weizhebu 9,〕 5 I 3,27 1 2Gr02 1 J, 50] 1 1 publisher 1! 2 1 1 | 50 1 1 _ 1 1 1 r; 丨 30 iT Mixture 6 2 in the tank. 1 3.00 | 49, commit 1 -0,93 i] 7,28 1, 30,]. ~ ”· 3 fiber those | 2.?0 I ^ 8,5J. | 1. 06 1 17,53 [30. ^ 7 Γ 1 publisher 1 | 30 1-1 1 35 0,5 1 1 i 12,5 | 1 mixture 7 2 in the tank | 29,36 | 35.-13 | 0 , 5 ^ 1] 2,76 | 1 3 suspected dimensionality | 29,30 1 I .3 already .52 1 I 1 0,47 1 1 | 1 P.2.28 I 1 1 publisher | 65 po 1 〇1】 0 | 5 1 Mixture 8 2 in the tank | 65,60 J9.79 I -0.0 ^ 1 D.B9 | 4 # 95 1 3 fiber 1 1 〇4, J 9 J 3 1 -0.2B 1 9,55 | 4,9G 1 1 17-^ ^ Binding ^ Ling (please read the precautions on the back before filling in this page) This paper size is applicable to the Chinese National Standard Falcon (CNS) A4 specification (210X 297 mm) ^ 20682 A7 B7 5. Description of invention () —
35躲 ¥: oiNS35 hide ¥: oiNS
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Has ITG*6tIs't •卜3 15-ε 10*st7 〇口 pn 5 69 εσ, 02 S 【 必一 ζ C9 ia¥-6i 二：ς· ι 9-ε 134 ε 〔-9卜·？ 9-GZ S Γ·?/ί 9ς 9【-3φ01 勺/ζε S,6V St7 6: 9G 1 T9 Λ LI ε 幻 Εσ, οε ς'卜 t --1σ>·Η 08 ο^·10⑺ ε 66 Φί7 90*C9 9-6T Λ>ε* i Δ6·ςζ 6^-6^ G-6C s s-l; 匁 ε G-ςζ101-1εε‘ζ®εςί7·σ,Ι7 0t7 61^9.51:τ ..〔ε·【 ^ 9··ι-ζε ς^-ε 61 ---；---^---i -种衣— (請先Μ讀背面之注意事項再填寫本頁) 訂 線 經濟部中央標準局員工消費合作社印裂Has ITG * 6tIs't • Bu 3 15-ε 10 * st7 口 口 pn 5 69 εσ, 02 S 【Must be one ζ C9 ia ¥ -6i 2: ς · ι 9-ε 134 ε 〔-9 Bu ·? 9-GZ S Γ ·? / Ί 9ς 9 【-3φ01 scoop / ζε S, 6V St7 6: 9G 1 T9 Λ LI ε 幻 Εσ, οε ς '卜 t --1σ > · Η 08 ο ^ · 10⑺ ε 66 Φί7 90 * C9 9-6T Λ > ε * i Δ6 · ςζ 6 ^ -6 ^ G-6C s sl; 匁 ε G-ςζ101-1εε'ζ®εςί7 · σ, Ι7 0t7 61 ^ 9.51: τ .. ( ε · 【^ 9 ·· ι-ζε ς ^ -ε 61 ---; --- ^ --- i -seed coat— (please read the precautions on the back first and then fill out this page). Bureau of Standards and Staff Consumer Cooperative
0S G,oe ς- °·ςα,ς\ς °'ος ^&πκ δ 1 本纸張尺度適用中國國家標隼（CMS ) A4規格（210X297公董） 經濟部中央櫺準扃貝工消費合作社印製 A7 乂 — — B7 五、發明説明（） 一 選定之置換期間為100秒*因此，整個循環捋續40分鏡 。各俚參考流速如下（在150*C下者）： 溶劑 ： 8.635 ctt3/ii η 區 1: 4 2 . 395 CBs/ain 萃取物 ： 8·44 cia3/丨 ίη 區 2 : 33. 955 CB3/ain 進料 ： 5.415 cjd3/· i n @3:39. 37 c*3/ain 萃餘物 ： 5.61 cm3/η i n S 4： 33. 76 ci3/«in 测定之流速如下： 溶劑 ： 8,61 c»3/ain* 即 10.545 g/期間 萃取物 ： 8 · 4 0 c a 3 / b i n * 即 1 0 · 2 8 7 g/期問 進料 ： 5.4 4 5 c b 3 / π i n ，即 6.669 g/期間 萃餘物 ： 5 . 59 cm3/tin* 即 6.856 g/期間 損失率 ： 0.065 cm3/Birf ，即 0.0 71 g/期間（即0.46X) 簞元在S定狀態搡作24小時後測得之姐成如下： 萃取物 萃餘物 甲苯 :85.353X 甲苯 ：16.168X 乙笨 :0.179X 乙笨 ：10.534X 對二甲苯 ：14.356X 對二甲苯 ：0.270JK 間二甲笨 :0.048X 間二甲苯 ·· 49.041X 鄰二甲笨 :0.014X 鄰二甲苯 ：13.987X 利用配置於内回路之三倜感應器， 每隔13分鐘及30秒觀 察一次完全之濃度分佈Η; 該分佈圖頭示於圓3 。但須知 ，藉重疊三倨感應器各提供之分ffl圖 *會有相當於約10秒 之稍撤移位 。另外，發生在參考號4_ 之間二甲笨尖峰之開 始顯示區4 内之流速過低， 此由過高水準之溶劑消耗可看 -19 - 本纸張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -I n n - n I - I ^ - - - n n n T n n I n n l · 一 J-d 一·" (請先閲讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消費合作社印裝 A7 B7 五、發明説明（） 出。 奮俐3 : 採用上述設備及操作條件•將單元停止MR察四種再循 環流速之修正對灌度分佈圖之影響。 程序1 :在150Ό下之各届參考潦速如下： 溶劑 ：7.85 ci»3、in 區 1 : 42.395 (；·3/·ίη0S G, oe ς- ° · ςα, ς \ ς ° 'ος ^ & πκ δ 1 This paper scale is applicable to the Chinese National Standard Falcon (CMS) A4 specification (210X297 company director) Ministry of Economic Affairs Central Ministry of Economics Consumption of shellfish Printed by the cooperatives A7 乂-B7 V. Description of the invention (1) The selected replacement period is 100 seconds * Therefore, the entire cycle continues for 40 minutes. The reference flow rate of each slang is as follows (under 150 * C): Solvent: 8.635 ctt3 / ii η Zone 1: 4 2. 395 CBs / ain Extract: 8.44 cia3 / 丨 ίη Zone 2: 33. 955 CB3 / ain Feed: 5.415 cjd3 / · in @ 3: 39. 37 c * 3 / ain Raffinate: 5.61 cm3 / η in S 4: 33. 76 ci3 / «in The measured flow rate is as follows: Solvent: 8,61 c» 3 / ain * is 10.545 g / period extract: 8 · 4 0 ca 3 / bin * is 1 0 · 2 8 7 g / period feed: 5.4 4 5 cb 3 / π in, which is 6.669 g / period extraction Remainder: 5.59 cm3 / tin *, or 6.856 g / period loss rate: 0.065 cm3 / Birf, or 0.0 71 g / period (i.e. 0.46X) As follows: Extraction Raffinate Toluene: 85.353X Toluene: 16.168X Ethylbenzene: 0.179X Ethylbenzene: 10.534X p-xylene: 14.356X p-xylene: 0.270JK m-dimethylbenzene: 0.048X m-xylene 49.041 X o-Dimethylbenzyl: 0.014X o-xylene: 13.987X Use the three sensors arranged in the internal circuit to observe the complete concentration distribution Η every 13 minutes and 30 seconds; Round 3. However, it should be noted that by overlapping the three points provided by the three sensors, there will be a slight shift of about 10 seconds. In addition, the flow rate in the display area 4 at the beginning of the peak of Erjiaben peak between reference numbers 4_ is too low, which can be seen from the excessively high level of solvent consumption. -19-This paper scale is applicable to the Chinese National Standard (CNS) A4 specification (210X297mm) -I nn-n I-I ^---nnn T nn I nnl · one Jd one · " (please read the precautions on the back before filling in this page) Employee Consumer Cooperative of Central Bureau of Standards, Ministry of Economic Affairs Printed A7 B7 5. Description of the invention (). Fenli 3: Using the above equipment and operating conditions • Stop the unit and check the effects of four types of recirculation flow rate corrections on the irrigation profile. Procedure 1: The reference speed of each session under 150Ό is as follows: Solvent: 7.85 ci »3, in zone 1: 42.395 (; · 3 / · ίη
萃取物：8.44 CBs/*in @ 2 : 33.955 (；·3/β i η 進料 ：5. 415 ca3/iin 區 3 : 39.37 cb3/bU 萃餘物：4.825 cm3/懸 in 區 4: 34.545 χρ3/·ίη 損失率占全部輸入之約0.5 % »單元搡作2 4小時後測定 之姐成如下 ♦ f 萃取物 - 萃餘物 甲笨 ：85.026X 甲笨 ：16.514X 乙笨 :0.217X 乙笨 ：12.042X 對二甲苯 ：14.303X 對二甲苯 ：0.169X 間二甲苯 ：0.264X 間二甲笨 ：55.335* 鄰二甲苯 ：0.090X 鄰二甲苯 :15.940* 利用配置於内回路之三俚感應器，每隔13分鑪又20秒觀 察一完全之濃度分佈圈。須知此時，間二甲苯尖峰之開始 事實上在參考號1 (Β 4)。相對照地·令人意外的是•間 二甲笨濃度之平頂僅發生在54.25 %。另一方面，需要等 待約15個循環，以便間二甲苯之0:25%之連鑛底部沿整俚 管柱建立。當目標為缠中鈍度（95¾ )之萃取物，》後再如 法國專利91/1 1004结晶純化時*必須尋求該型之濃度分佈 -20 - 本纸張尺度適用中國國家標牟（CNS ) A4規格（210X297公釐） | ； 一，装 I I I I I 訂— I J 务 (請先閏讀背面之注意事項再填寫本頁) A7 B7 經濟部中央標準局負工消费合作社印裂 五、發明説明（） 圖。區1内之分佈圈與實例2及3 (程序2 )之籣箪比較即 可顯示該區內之流速是否裔要改變。 程序2 ;在150P下之各個參考流速如下： 溶劑 ：8.635 ca3/· i η 區1 : 42.395 CB3/·i 萃取物 ：8.44 cb3/·i η 區2 : 33.955 •c·3/· i 進料 ：5.995 c·3/·i η 區3: 39.95 c·3/·i n 萃餘物 ：6.19 cm3/·i η g 4: 33.76 c·3/·i n 損失率占全部_入之約0.5 %。在單元之穩定狀態搡作 24小時後浦定之姐成如下：Extract: 8.44 CBs / * in @ 2: 33.955 (; · 3 / β i η Feed: 5.415 ca3 / iin zone 3: 39.37 cb3 / bU Raffinate: 4.825 cm3 / suspension zone 4: 34.545 χρ3 / · Ίη loss rate accounts for about 0.5% of all inputs. The unit ’s measurement after 2 to 4 hours is as follows. ♦ f Extraction-Raffinate Abenben: 85.026X Abenben: 16.514X Abenben: 0.217X Abenben : 12.042X p-xylene: 14.303X p-xylene: 0.169X m-xylene: 0.264X m-xylene: 55.335 * o-xylene: 0.090X o-xylene: 15.940 * using the three-sensor sensor configured in the inner circuit ， Observe a complete concentration distribution circle every 13 minutes and another 20 seconds. Note that at this time, the beginning of the m-xylene spike is actually at reference number 1 (Β 4). Comparatively, the surprise is that The flat top of the concentration of Jiaben only occurs at 54.25%. On the other hand, it is necessary to wait for about 15 cycles so that the bottom of the continuous ore of 0: 25% of m-xylene is established along the entire stub. When the target is entanglement blunt (95¾) extract, after the crystallization purification of French patent 91/1 1004 * must seek the concentration distribution of this type -20-this The Zhang scale applies to China National Standards (CNS) A4 specification (210X297mm) |; First, install IIIII order-IJ business (please read the notes on the back side before filling this page) A7 B7 Negative work of Central Standards Bureau of Ministry of Economic Affairs Printed by the consumer cooperative V. Description of the invention () Figure. The distribution circle in zone 1 can be compared with the examples 2 and 3 (program 2) to show whether the flow velocity in the zone is to be changed. Procedure 2; under 150P The respective reference flow rates are as follows: Solvent: 8.635 ca3 / · i η zone 1: 42.395 CB3 / · i extract: 8.44 cb3 / · i η zone 2: 33.955 • c · 3 / · i feed: 5.995 c · 3 / · I η area 3: 39.95 c · 3 / · in raffinate: 6.19 cm3 / · i η g 4: 33.76 c · 3 / · in The loss rate accounts for about 0.5% of the total input. In the stable state of the unit After 24 hours, the sister of Puding became as follows:
萃取物 萃餘物 甲笨 :84.430X 甲苯 ：26.777X 乙苯 ：0.430X '乙笨 ：10.188X 對二甲苯 ：15.158X 對二甲笨 :1.083* 間二甲笨 :0.046X 間二甲苯 :48.161X 鄰二甲苯 :0.016X 鄰二甲笨 ：13.79U 利用配置於內回路之三儷感應器*每隔13分鐘又20秒费 察澹度分佈困。此次，在乙苯灌度分佈圈安定化之前，箱 有40個Κ上循環，而有關對二甲苯之安定化之狀況則很快 達成（約10俚循環）。相對於程序1 ，因此發現區3内流 速之增加並非有利（產率及鈍度均下降）。另一方面*純度 之劣化緩慢，因此可及早反應至乙苯存料之增加· Μ致可 防止萃取物被乙笨所污染。圖5 ©示在實例2(1)及實例 3(2)之程序2之情況下乙苯之分佈圖-，其他物種之分佈· 僅略加修改。 -21 - 本纸張尺度適用中國國家標準（CNS ) Α4規格（210Χ 297公釐） -------1--『裝------訂-----~-|線 (請先Μ讀背面之注意事項再填寫本頁) A7 B7 經濟部中央標準局員工消费合作社印裝 五、發明説明（） 箱庠:在150X：下之各值參考流速如下： 溶劑 ：8.635 cB3/dn 匿 1 : 42.395 (；·3/·ίη 萃取物 ：9.02 cm3/Bin E 2 : 33.375 c·3/· i η 進料 ：5· 995 (；·3/·ίη 區 3 : 39.37 <ϊ·3/·ίη 萃 餘 物 5. 64 c 3/* i η 區 4 : 3 3 · 7 6 c · 3 / 麗 i n 撗 失 率 占 全 部轤 入之約 0· 5 %。在單 元 穩定狀想搡 作 2 4小 時 後 m 定 之姐 成如下 * 萃 取物 萃餘物 甲 笨 ：82 .357Χ 甲苯 ：22.385* 乙 苯 ：2. 043Χ 乙苯 ：8.588X 對 二 甲 苯 ：14 .557* 對二甲笨 ：0.578X 間 二 甲 苯 :0.048X * 間二甲笨 :53.109X 鄰 二 甲 苯 ：0. 015Χ 鄰二甲笨· :15.340X 利 用 配 置 於 内回 路之三 m 感應器•每 ffi 13分鐘又20秒 可 觀 察 濃 度 分 佈 圈。 相對於 程 序2 ，濃度 分 佈Η巳充分 修 改 » 且 在 轉 移 狀 況時 ，萃取 物 內對二甲笨 之 穰度在約14 .596 安 定 化 前 增 至 18¾ 。對於 超 過48小時之 期 間*乙苯潇 度 分 佈 圓 會 改 變 9 且令 人吃驚 的 是區3之平 頂 其濃度水準 較 所 有 其 他 程 序 者 更高 ，而萃 餘 物内乙笨之 濃 度水準則由 10 .296 落 至 8. 6 % 。圖6 濃 度分佈圔之 篛 單視覺檢驗 即 足 以 看 出 區 1 内 流速 之增加 可 防止對二甲 苯 因萃餘物而 失 去 〇 在 百 前 情 況 •在 少於1 小 時30戎内· 區 4内可截獲 對 二 甲 笨 0 僅 藉 本 發明 觀察濃 度 分佈圓之變 異 可迅速對良 好 參 數作出反應。 -22 - 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） | ： f 裝 訂 y ^ (請先閱讀背面之注意事項再填寫本頁) 經濟部中央標隼局員工消费合作社印裝 ^2〇β§2 Α7 _'___ Β7_ 五、發明説明（） 一 g序4:在150X3下之各届參考流速如下： 溶劑 ：8.635 cn3/«in Si： 42.735 c·3/· ί η 萃取物 ：8.44 cn3/ain 區 2 : 34.295 c ·3/· i η 進料 ：5.415 <:·3/·ίη 區 3: 39.71 ci3/^in 萃餘物：5.61 (：·3/·ίη 區 4: 34. 10 caa/^in 損失率占全部_入之約0.5 %。在單元之檯定狀態搡作 24小時後测定之姐成如下： 萃取物 萃餘物 甲苯 ：86.989Χ 甲苯 ：23.950Χ 乙笨 ：0.043Χ 乙笨 :10.705* 對二甲苯 :12.&88Χ 對二甲苯 ：2.355Χ 間二甲苯 ：0.045Χ ~間二甲笨 :40.008Χ 鄰二甲苯 ：0.015Χ 鄰二甲笨 ：13.992Χ 利用配置於内回路之三届感應器*毎隔13分鑪又20秒観 察濃度分佈Η。相對於程序3 *分佈圖已經相當大修正， 且在操作之過渡期間，萃餘物内乙笨之量在約10.7%安定 化前升至18%。再次乙苯分佈圓巳完全修正•而對二甲苯 分佈園則回至，相當接近實例2之型式。在此程序中•僅 利用修正再循瑁之流速可得鈍度高於99.2%之對二甲苯。 當依照濃度分佈園之變異時•參考值不會變•儘管有似乎 可能警人之萃餘物姐成之變異•因為此等分佈圈已被修正 接近所欲之分佈圓：如画7所示C此處本發明可维持參考 值*不顳流出物组成之相當大變異。_依照先前技蕕（僅流 出物之分析），參考值會被不烴意地修正。 -23 - 本紙張尺度適用中國國家橾準（CNS ) Α4说格（210Χ 297公釐） -------^---一·裝------訂-----γ 線 (請先閱讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消费合作社印裝 A7 B7__ 五、發明説明（） - 苷例4 : 在底部製造鄰二甲笨及在頭部製造間二甲苯、對二甲笨 與乙苯之混合物之蒸皤管柱，包含280片實板。視其姐成 而定，可在第110片板或第135片板導人進料。再沸器被 視為第282片板而回流球形焼瓶視為第一片板。 管柱裝有二種進料，具有下列姐成： 異構化物 Tatoray單元流出物Extract Raffinate Abenben: 84.430X Toluene: 26.777X Ethylbenzene: 0.430X 'Ethanben: 10.188X p-xylene: 15.158X p-dimethylbenzen: 1.083 * m-benzenben: 0.046X m-xylene: 48.161 X o-xylene: 0.016X o-xylene stupid: 13.79U Use the three-liquid sensor arranged in the inner circuit * It is difficult to check the distribution of temperature every 13 minutes and 20 seconds. This time, before the stabilization of the ethylbenzene irrigation distribution circle, there were 40 K cycles in the tank, and the situation regarding the stabilization of p-xylene was quickly reached (about 10 slam cycles). Relative to procedure 1, it is found that the increase in flow rate in zone 3 is not favorable (both yield and bluntness decrease). On the other hand, the deterioration of purity is slow, so it can be reacted to the increase of ethylbenzene stock early. M can prevent the extract from being contaminated by ethyl stupid. Figure 5 © shows the distribution of ethylbenzene in the case of procedure 2 of Example 2 (1) and Example 3 (2)-, distribution of other species · Only slightly modified. -21-This paper scale is applicable to the Chinese National Standard (CNS) Α4 specification (210Χ 297 mm) ------- 1-"installation ------ order ----- ~-| line (Please read the precautions on the back first and then fill out this page) A7 B7 Printed by the Employees ’Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention () Box: At 150X: the reference flow rate for each value is as follows: Solvent: 8.635 cB3 / dn An 1: 42.395 (; · 3 / · ίη Extract: 9.02 cm3 / Bin E 2: 33.375 c · 3 / · i η Feed: 5.995 (; · 3 / · ίη Zone 3: 39.37 < ϊ · 3 / · ίη Raffinate 5. 64 c 3 / * i η Zone 4: 3 3 · 7 6 c · 3 / Li in the loss rate accounts for about 0.5% of the total entrants. It is stable in the unit After 2 to 4 hours, I want to make the sister as follows: * The extract residue is stupid: 82.357X toluene: 22.385 * ethylbenzene: 2.043X ethylbenzene: 8.588X p-xylene: 14.557 * p-dimethyl Stupid: 0.578X Meta-xylene: 0.048X * Meta-dimethyl stupid: 53.109X o-Xylene: 0.015X o-Dimethyl stupid ·: 15.340X Use the configuration in the inner back Road No. 3m sensor • The concentration distribution circle can be observed every 13 minutes and 20 seconds per ffi. Compared with program 2, the concentration distribution Η has been fully modified »and in the case of transfer conditions, the degree of dimethylbenzene in the extract is about 14.596 Increased to 18¾ before stabilization. For more than 48 hours * the ethylbenzene distribution circle will change by 9 and surprisingly, the concentration level of the flat top of zone 3 is higher than that of all other programs. The concentration water standard for ethyl stupid in the residue fell from 10.296 to 8.6%. Figure 6 The visual inspection of the concentration distribution is sufficient to see that the increase in the flow rate in zone 1 can prevent paraxylene from being caused by the residue. Lost 〇 in a hundred years ago • Within less than 1 hour and 30 hours • Zone 4 can be intercepted for dimethyl sulfonate 0. The variation of the concentration distribution circle observed by the present invention alone can quickly respond to good parameters. -22-This paper scale is applicable to the Chinese National Standard (CNS) A4 specification (210X 297mm) |: f Binding ^ (Please read the notes on the back before filling this page) Printed by the Employee Consumer Cooperative of the Central Standard Falcon Bureau of the Ministry of Economic Affairs Install ^ 2〇β§2 Α7 _'___ Β7_ V. Description of invention () One g sequence 4: The reference flow rate for each session under 150X3 is as follows: Solvent: 8.635 cn3 / «in Si: 42.735 c · 3 / · ί η Extract: 8.44 cn3 / ain Zone 2: 34.295 c · 3 / · i η Feed: 5.415 <: · 3 / · ίη Zone 3: 39.71 ci3 / ^ in Raffinate: 5.61 (: · 3 / · ίη Zone 4: 34. 10 caa / ^ in loss rate accounted for about 0.5% of the total input. After 24 hours of operation in the unit's stationary state, the measured results are as follows: Extraction Raffinate Toluene: 86.989X Toluene: 23.950 Χ Ethylene: 0.043 Χ Ethylene: 10.705 * p-xylene: 12. & 88X p-xylene: 2.355X meta-xylene: 0.045Χ ~ meta-dimethyl stupid: 40.008Χ o-xylene: 0.015Χ o-dimethyl stupid ： 13.992Χ Use the three-phase sensor arranged in the inner circuit * to observe the concentration distribution Η every 13 minutes and another 20 seconds. Compared with the program 3 * the distribution map is already equivalent Major revision, and during the transition period of the operation, the amount of ethyl stupid in the raffinate rose to 18% before the stabilization of about 10.7%. Once again, the ethylbenzene distribution was completely revised. The paraxylene distribution garden returned to the equivalent It is close to the type of Example 2. In this procedure, only using the flow rate of the re-circulation stream can obtain para-xylene with a bluntness higher than 99.2%. When the variation is based on the concentration distribution, the reference value will not change. May be the variation of the policeman's raffinate • Because these distribution circles have been corrected close to the desired distribution circle: as shown in Figure 7 C here the invention can maintain the reference value * The composition of the temporal effluent is quite large Variations. _According to the previous technique (analysis of effluent only), the reference value will be corrected unintentionally. -23-This paper scale is applicable to the Chinese National Standard (CNS) Α4 specification (210Χ 297 mm) --- ---- ^ --- 一 · 装 ------ 定 ----- γ line (please read the precautions on the back before filling in this page) Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs Printed A7 B7__ 5. Description of the invention ()-Glycoside Example 4: Manufacture of o-dimethyl stupid at the bottom and m-xylene and p-dioxin at the head The steamed column of a mixture of Jiaben and ethylbenzene contains 280 solid plates. Depending on the success of its sister, it can be fed into the 110th or 135th plate. The reboiler is regarded as the 282nd plate. The plate and the recirculating spherical bake bottle are regarded as the first plate. The column is equipped with two kinds of feeds and has the following successes: Isomers Tatoray unit effluent
EB 10.2X 4.0X PX 20.45J； 22.5%EB 10.2X 4.0X PX 20.45J; 22.5%
MX 48.10¾ 50. IXMX 48.10¾ 50. IX
OX 20.5X 23.4X 各種雑質 0.75X * 為了回應可變性箱求之危除•蒸《管柱可裝有二種進料 之一及兩種進料之混合物。該管柱之調節係依照先前技《 利用下面調節效應完成：監測進料流速、監測管柱頭之回 流流速、監測排出鎇出液之回流燒瓶之高度、監測排出鄰 二甲苯之再沸器之高度，藉可在第225片板上感應之湛度 監測進入爐内之燃堍氣體之量。每日監测饑出液之姐成及 鄰二甲苯可確保鄰二甲笨之纯度為98.5%及產率自80至 90%不等。該管柱設有四個光學感應器•供管柱第280片 、255片、120片及第2片板上姐成之賁時分析。另外， 動力模擬棋型以加速時間揲作，蒎可計算管柱對姐成改變 之回應。將有鼷直正姐成之數據與計_算之姐成比較•且依 照實時觀察並計算之姐成計算再沸器之热艙出、回流速率 -24 - 本紙張尺度適用中國國家標準（CNS ) Α4規格（2丨〇><297公釐） I I I -I - - - - - - - I ii ( I- I 1 n I I - 1 - I — -- - In ^^1 (請先Μ讀背面之注意事項再填寫本頁) A7 -、 · · B7 五、發明説明（） — 及進料加入管柱之高度。鄰二甲苯之平均純度水準因此自 98.5%變成98.9%，而產率在93與95%之間波動，此在瞬 間操作狀態時，不會中斷或再循環。 -------：--「-裝------訂------^線 - (請先Μ讀背面之注意事項再填寫本瓦) 經濟部中央標準局員工消費合作社印製 -25 - 本纸張尺度適用中囡國家標準（CNS ) Α4規格（210Χ 297公釐）OX 20.5X 23.4X Various types of refractory materials 0.75X * In response to the danger of variability box request • Steam "The column can be equipped with one of the two feeds and a mixture of the two feeds. The adjustment of the column is done according to the previous technique "Using the following adjustment effects: monitoring the feed flow rate, monitoring the reflux flow rate of the column head, monitoring the height of the reflux flask discharging the effluent, monitoring the height of the reboiler discharging o-xylene It can monitor the amount of gas burned into the furnace by the concentration induced on the 225th board. Daily monitoring of the sister and o-xylene of the hungry fluid can ensure that the purity of o-dimethyl stupid is 98.5% and the yield varies from 80 to 90%. The column is equipped with four optical sensors. It is used to analyze the 280th, 255th, 120th, and second parts of the column. In addition, the dynamic simulation of the chess pattern works with acceleration time, and pin can calculate the response of the column to the sister change. Comparing the data of Youzhi Zhizheng Cheng and the calculation of the calculation of the sister, and calculating the reboiler hot compartment outflow and reflux rate according to the real-time observation and calculation of the sister calculation-this paper scale is applicable to the Chinese National Standard (CNS) Α4 specification (2 丨 〇 < 297mm) III -I-------I ii (I- I 1 n II-1-I —--In ^^ 1 (please read first (Notes on the back and then fill in this page) A7-, · · B7 V. Description of invention () — and the height of the feed into the column. The average purity level of o-xylene has therefore changed from 98.5% to 98.9%, and the yield is Fluctuation between 93 and 95%, this will not be interrupted or recirculated during the instantaneous operation state. -------:-"-installed ------ ordered ------ ^ line -(Please read the precautions on the back before filling in this tile) Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs -25-This paper scale is applicable to the Chinese National Standard (CNS) Α4 specification (210Χ 297 mm)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW83105961A TW320682B (en) | 1994-06-30 | 1994-06-30 | Method and apparatus for regulating a process for the separation of isomers of aromatic hydrocarbons having from 8 to 10 carbon atoms by a monochromatic light signal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW83105961A TW320682B (en) | 1994-06-30 | 1994-06-30 | Method and apparatus for regulating a process for the separation of isomers of aromatic hydrocarbons having from 8 to 10 carbon atoms by a monochromatic light signal |
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| Application Number | Title | Priority Date | Filing Date |
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| TW83105961A TW320682B (en) | 1994-06-30 | 1994-06-30 | Method and apparatus for regulating a process for the separation of isomers of aromatic hydrocarbons having from 8 to 10 carbon atoms by a monochromatic light signal |
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- 1994-06-30 TW TW83105961A patent/TW320682B/en not_active IP Right Cessation
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