TW386041B - Method for controlling with precision a process for separating constituents of a mixture, in a simulated moving bed separation system - Google Patents

Method for controlling with precision a process for separating constituents of a mixture, in a simulated moving bed separation system Download PDF

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TW386041B
TW386041B TW87106265A TW87106265A TW386041B TW 386041 B TW386041 B TW 386041B TW 87106265 A TW87106265 A TW 87106265A TW 87106265 A TW87106265 A TW 87106265A TW 386041 B TW386041 B TW 386041B
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ratio
value
patent application
variables
fluid
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TW87106265A
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Chinese (zh)
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Nicolas Couenne
Pascal Duchene
Gerard Hotier
Dominique Humeau
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Inst Francais Du Petrole
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Description

第87106265號專利申請案 中文說明書修正頁(88年11月、 五、發明説明(13) 該計算演算法包括真實移動床單元之非線性物理模式, 其能夠計算比值(如段II中所定義),所以被控制變數可以 在事先得到固定之值。該計算方法係費力、非t迅速且暗 示在線上足夠之測量是可以的。 a) 比值計算原則 ; 將由熟習該項技藝之人士所適當選擇之數目為m之式(〇 所給之形式之被控制變數限制於區段中,其中m係小於或 等於η ’即一組相鄰包括一或多個區域之階段,其中係定義 η偏比值。藉由定義統計模式之代數式以及在區段之端 點處之液相中之濃度之可得測量,這些m個被控制變數能 夠計算m個比值或含有(n-m)個參數之這些比值之m種合併 〇 b) 對4-區單元之純度計茸籁例 純度ξρ係只能從萃取物(Xert)之組成之認知中定出: gp = F(Xert) 選擇一包含區域1之部份以及區域2之部份之區段(圖3), 其中2個比值因此可定出。比值r 1、在端點處之液相中所 有组份之濃度Xe與Xs以及純度之設定值(被控制變數)之認 知能夠去計算比值R2。 實際上,從式(7)且對組份i (指數m表示真實之測量值), 我們可以窝出: -在階段e+1 :Revised page of Chinese Specification for Patent Application No. 87106265 (November 88, V. Description of Invention (13) The calculation algorithm includes a non-linear physical model of a real moving bed unit, which can calculate the ratio (as defined in paragraph II) Therefore, the controlled variable can get a fixed value in advance. The calculation method is laborious, not fast and implies that sufficient measurements are available online. A) The principle of ratio calculation; it will be appropriately selected by those skilled in the art The number of equations in the form of m (0 is limited to the controlled variables in the form of m, where m is less than or equal to η ', that is, a group of adjacent stages including one or more regions, where η is a partial ratio. By defining an algebraic expression of the statistical model and the available measurement of the concentration in the liquid phase at the endpoints of the segment, these m controlled variables can calculate m ratios or m of these ratios containing (nm) parameters Merging 〇b) The purity of the 4-zone unit is calculated. For example, the purity ξρ can only be determined from the knowledge of the composition of the extract (Xert): gp = F (Xert) Select a part that contains region 1 and The segment portion of domain 2 (FIG. 3), wherein the two ratios thus fix. The ratio r1. The knowledge of the concentration Xe and Xs of all components in the liquid phase at the endpoints and the knowledge of the setpoints (controlled variables) of purity can be used to calculate the ratio R2. In fact, from equation (7) and for component i (the index m represents the true measured value), we can find out:-at stage e + 1:

Ri(xmi,e-Xi,e+i) + (yi,e+ryi,e+i)+K(Xi,e+2-Xi,e+1)=0 -16- 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) 一請先閲讀背面之注意事項符填寫本寅〕 ,ίτ 經濟部中央標準局員工消費合作杜印裝 Α7 Β7 經濟部中央標準局員工消費合作社印製 五、發明説明(彳) 發明領域 本發明乃關於從不連續濃度與流量測量以精確地控制在 模擬移動床分離系統中用以分離混合物之組份之製程之方 法ύ本方法尤其是使用於芳香族烴類之分離。 發明背景** 在工業上,有許多種基於選擇性地吸附流體混合物之數' 種成份中之至少一種之連續分離方法,尤其是已知爲模擬 疋相色層分析法者,其中係使用到在液體、氣體或超臨界 混合物之#在下,某些多孔性固體顯著地保留f較多或較少 混合物之各個组份之性質。 ^ 基於色層分析法之分離或分餾方法最通常係在含有一組 塔柱或串聯連接之塔柱分部、以形成,迴路之設備中施行 。用於欲分離之混合物和溶劑或脱g劑之注入點、以及用 於萃取物與萃餘物之流體萆取點將定出不同區域之範圍、 且沿著此迴路分佈。相同之液體流通過所有之塔柱或相同 區域之塔柱分部。 此設裱最通常係由四個主要之區域所構成。不過,某些 只具有二個區域(在此例子中,於萃餘物取出點與溶劑注 入點間所包含之區域被省略)。亦有設備係具有五個區域 的’其中從溶劑中所分離出之萃取物之部份被再注入萃取 物取出點與進料注入點間.。其他可能包括五至七個區域,, 其中允許第二流體去沖洗#連輸送數種流體之管線;,以防 止污染。 以已決定顆粒大小之多孔性固體形成固定相。欲分離之 __________ * 4 - 本紙張尺度適用中國國家標準(CNS〉M規格(2】〇 χ Μ?公隻〉 (請先閱讀背面之注意事項再填寫本頁) '装. 訂 經濟部中央標隼局員工消費合作礼印製 A7 __一 _ B7_____ 五、發明説明(2 ) 混合物係飼入塔柱中,然後藉一載流體或脱附劑以排代, 且各组份根據其是否被固定相更顯著地或較不顯著地保留 ,以接連地流出。 .在.眞實之反向流製程中(.圖1 ),,穩定與固定之濃.度 分佈在分離塔柱1中發展,其中進料“ A+B、洗脱物s之注入 點以及萃取物EA與萃餘物RB之取出點之位置仍維持固定 。該吸附固體3與液體2以反向流之方式循環。同時置放於 塔柱處(在區I與區IV之連接處)之一囪體運送系統與循環 泵P分別允許將固體從底部送至頂部且相反地,將液體從頂 部送至底部,其中存在於液體以及固體中之唯一組份爲洗 脱載流體。 已知爲模擬移動床方法之製程可允許避免在眞實移動床 方法中固有之主要困難,其包括正^地循環該固體相而不 會產生磨耗以及不會顯著地與增加與固定床有關之床之孔 隙度。爲了模擬其之排代作用,固體保放置於串聯排列之 某些數目η之固定床中(通常4 s n g 24),且該濃度分佈係 在本質i均勻之速率下於整個閉迴路中被誹代。 在實際上,注入點與取出點之連續變換係藉旋轉閥或更 簡單地藉一组適當控制之開關閥以進行。各個進入-離去 流動在给定之方向於每一階段中進行之循環變換,相當於 模擬固體吸附劑在反方向上之排代。 , 反向或同向流模擬移動床色層分析法係例如描述於美國 專利罘2,985,589號或美國專利第4,4〇2,832號中。 一用於將含有至少二種組份之進料、在至少一個洗脱劑 _ -5- 本紙張尺度適用中國國家標準(CNS ) A4規格(2〗0X297i5^ ---— 1^^ 1» -·-1·— - - 111-. - -II I: 1 11 I-I - - - -I —— ------ ' I f r .:¾ 、-'口 -.、 (諳先閱讀背面之注意事項再填寫本頁) 、 A7 A7 經濟部中央標準局員工消費合作社印製 五、發明説明( ,下分離成至少二個餘份之系統,其通常含 :4S“24)串聯安裝之_路色層分析塔柱或塔柱區通 其中係循環加磨之液體、超臨界或氣體混合物,該迴路 有至少-個進料注入流、至少一個殊脫劑注入流'至少: =取物取出流以及至少―個萃餘&取出流,該组份主: 在萃取物或在萃餘物中獲得係較佳的。 主要之入口流量爲進料流量與洗脱劑流量,出口流量/ 萃取物流量。該萃餘物係在屦力控制下取出,萃餘物之: I係等於入口流量之總和減去萃取物流量。除了這些控: 〈流量外’其亦有一控制之循環流量,其値與、給定之 間下泵之位置有關。根據欲進行之分離種類以計算此四個 園繞在床周圍之流動之每—插之相對位置,以得到一 之行爲且因此定出圖i所示之方法G子中之四個不同區 域0 美國專利第?d57:260粟與11^4貼.號描述一用於分 離组份之混合物之模擬移動床系統之控制方法,其含有二 個迴路互相連#之多塔床塔柱,其+至少一個特色爲控制 組份之純度或其之產量或二者之合併。該方法包_量在 塔柱相互連接之管路中循環之各個混合物之组份之濃度, 特別是藉近紅外線光譜,且使甩一多變數迴歸式或神=網 路式之·反覆調整演算法,其係傾向於減小特性之眞實値與_ 設定値間之差異。此處所用之演算法爲••黑盒子"式,其具 有此種方法所具有之缺點:可觀之實施時間,因爲結果只 月b在多次之測萬後獲得,其只能在測試之領域中使用且其 6 本紙張尺度適用中國國家標隼(CNS ) A4規格(210X297公釐) f辞先聞讀背面之注意事項再填窍本頁」 策 、-* A7 B7 經濟部中央標準局員工消費合作社印製 五、發明説明(4 只能得到很差之精確度。 在下又中,標示下逑之用語: -笋控制變數:必須闳宁从4. z l 1 ‘“ V 固定地接近預先決定好之設定值泛镦 數,且其顯示製程之平对冬叹疋値<變 ^純度、分離罕元對—给定组份之i率等; 知 -敏it—變―數:可以由操作者變 土描拉士、u ι数,例如流•量或允許 去模擬床 < 排代之閥變換期等 -接j彳變數·主要係作用於簞區 > 燃& ' .~了: 於皁5义變數,例如作用於包含 於β内之漠度分佛之部份。+此 以決定且傳送至操作變數。^^數係¥制演算法 。需要提醒的是,打算用於分離迴路運作之控制之高等製 私之目的係去計算一控制法則^立换阿、、β 利;則(在時間·^過程中所有操作 變數之値),保爲了 : < * %J1:星‘ii g卩去4算-能夠產朱_或多個已事先選擇之 控制變數之二個不同値間之轉移之控制法則,與 調整操作’即去計算—能_所有外部對製程之擾動儘可 能(事£或至少漸近)補償之控制法則,以使已事先選擇之 控制變數仍維持在準周定値。 在模擬移動床系統之例子中,對由於吸附劑之熱力學與 幾何參數(當然係對吸m劑性質之有限衰退)隨時間之進展 引起之擾動,亦可以以調整加以補償。 , 1¾些目標係藉欲用於分離根據本發明之循環流體混合物 組份之製程之自動控制方法以實現,其可以克服前述所提 之缺點。其並非基於"黑盒子”式之技街,而是基於更被控 本紙張尺度適用中國國家標隼(CNS ) A4規格(210Χ297公釐) Ί.Γ--------J衣-----—訂 (諳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費合作社印掣 A7 __B7 五、發明説明(5 ) — 制之方法,其係被分離方法之非線性模式所允許。 發明概述 根據本發明之方法係施用在用於分離组份之模擬移動床 系統(或單元)乏控-制上,其包括—由互相串聯連接且含有 吸附劑材料之塔床所組成之閉迴路'其係藉流體注入與取 出點劃分成數値區域、將流體注入迴路之裝置、將流體從 迴路中取出之裝覃、能夠樑擬塔床之反向排代之注入點與 取出點變換裝置、以及須ί量各個變數(例如濃度、流量、 閥變換期等)之裝置。其包含:~ -測量操作變數與某些組份之濃度,其係計算在至少等於2 之分離迴路上之許多點之銓制變數所需的; -從測量變數乏眞實値且藉使用一分離系統(可以是非線性 模式、或接近一給定運作點之線性;^式)工作之已決定模 式以決定各別標示比値之比値(Rk),其係在每一個不同之 區域中,介於流體流量(QK)與模擬吸附劑材料流量⑴“間 ,以將控制變數帶至或帶回已決定之設定植,以及 •從這比値(Rk)決定欲給至操作變數之値。 在含有包括η區且鄰接之階段之陣列之分離迴路區域上 ,其中定義出η個比値(Rk),該方法通常包含根襄流量(D) 與濃度値(X)定義出m相被控制變數(ξ ),其m値係小於或 等於η値,測量(至在非線性控制模式之例子中)在區段之~ 端點處於液相中之濃度(X)且決定m該比値(Rk)或該比値之 m合併,其含有(n-m)個參數。 根據一含有四個主要區域之分離迴路之具體實施例,例 -8 - 1紙張尺度^用中國國家標準(CNS ) A4規格(2ΐ〇χ29·7公釐) ' (請先閲讀背面之注意事項再填寫本頁) Λ衣· 、-° A7Ri (xmi, e-Xi, e + i) + (yi, e + ryi, e + i) + K (Xi, e + 2-Xi, e + 1) = 0 -16- This paper size applies to China Standard (CNS) A4 specification (210X297 mm) First, please read the note on the back to fill in the original text], ίτ Printed by the Central Consumers Bureau of the Ministry of Economic Affairs, printed Α7 Β7 Printed by the Consumer Cooperatives of the Central Bureau of Standards, Ministry of Economic Affairs 2. Description of the invention (彳) Field of the invention The present invention relates to a method for accurately controlling a process for separating components of a mixture in a simulated moving bed separation system from discrete concentration and flow measurement. This method is especially used for aromatics. Separation of hydrocarbons. BACKGROUND OF THE INVENTION ** In the industry, there are many continuous separation methods based on the selective adsorption of at least one of the components of a fluid mixture, especially those known as simulated pseudochromatographic analysis methods. Below a liquid, gas, or supercritical mixture, certain porous solids significantly retain the properties of the individual components of the mixture with more or less. ^ Separation or fractionation methods based on chromatographic analysis are most commonly performed in equipment that contains a set of columns or column sections connected in series to form a loop. The injection points for the mixture to be separated and the solvent or de-gelling agent, and the fluid extraction points for the extract and the raffinate will be defined in different areas and distributed along this circuit. The same liquid flow passes through all towers or tower divisions in the same area. This setup is most often composed of four main areas. However, some have only two regions (in this example, the region contained between the raffinate extraction point and the solvent injection point is omitted). There is also a device which has five areas where the portion of the extract separated from the solvent is re-injected between the extract extraction point and the feed injection point. Others may include five to seven zones, in which a second fluid is allowed to flush the pipelines that transport several fluids to prevent contamination. The stationary phase is formed from a porous solid whose particle size has been determined. __________ * 4-This paper size applies to Chinese national standards (CNS> M specifications (2) 〇χ M? 公 Only> (Please read the precautions on the back before filling out this page) A7 __ 一 _ B7_____ printed by the staff of the Bureau of Standards and Consumers V. Description of the invention (2) The mixture is fed into the tower and then replaced by a carrier fluid or desorbent, and each component is based on whether it is Retained by the stationary phase more or less significantly to flow out one after another. In the solid reverse flow process (Figure 1), the concentration and stability of the stationary and fixed phases are developed in the separation column 1 The positions of the feed point "A + B, the injection point of the eluate s, and the extraction point of the extract EA and the raffinate RB remain fixed. The adsorbed solid 3 and liquid 2 are circulated in a reverse flow. At the same time Placed on one of the towers (at the junction of Zone I and Zone IV), the mast transport system and the circulation pump P respectively allow solids to be sent from the bottom to the top and, conversely, liquids from the top to the bottom. The only component in liquids and solids is the eluent carrier fluid. The process of the moving bed method may allow to avoid the main difficulties inherent in the solid moving bed method, which include recycling the solid phase positively without abrasion and not significantly increasing the porosity of the bed associated with the fixed bed. In order to simulate its substitution effect, the solid is placed in a fixed bed of a certain number η arranged in series (usually 4 sng 24), and the concentration distribution is destroyed in the entire closed loop at a substantially uniform rate. In practice, the continuous conversion between the injection point and the withdrawal point is performed by means of a rotary valve or more simply by a set of appropriately controlled on-off valves. Each entry-exit flow cycles in a given direction in each stage The transformation is equivalent to simulating the replacement of the solid adsorbent in the reverse direction. The reverse or co-current simulated moving bed chromatography analysis system is described in, for example, US Patent No. 2,985,589 or US Patent No. 4,402,832. One is used to feed with at least two components in at least one eluent_ -5- This paper size applies Chinese National Standard (CNS) A4 specifications (2〗 0X297i5 ^ ---— 1 ^^ 1 » -·-1 ·---111-.--II I: 1 11 II----I —— ------ 'I fr.: ¾,-' 口-., (谙 Please read the precautions on the back before (Fill in this page), A7 A7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 5. The invention description (, the system is separated into at least two remaining systems, which usually contains: 4S "24) serial installation _ Road color layer analysis The column or column area communicates with the liquid, supercritical or gas mixture which is circulated and milled. The loop has at least one feed injection stream, at least one special agent injection stream, 'at least: = extraction extraction stream, and at least- A raffinate & extraction stream, the component mainly: better in the extract or in the raffinate. The main inlet flows are feed flow and eluent flow, and outlet flow / extract flow. The raffinate is taken out under the control of pressure, and the raffinate: I is equal to the sum of the inlet flow minus the extract flow. In addition to these controls: "In addition to flow," it also has a controlled circulating flow, which is related to the position of the lower pump at a given interval. According to the type of separation to be performed, calculate the relative position of each of the four circles of flow around the bed to obtain the behavior of one and thus determine four different regions in the method G shown in Figure i. US patent number? d57: 260 millet and 11 ^ 4 stickers. No. describes a control method of a simulated moving bed system for separating a mixture of components, which contains two multi-tower bed columns connected to each other #, and at least one of its features is Control the purity of a component or its yield or a combination of both. This method involves measuring the concentration of the components of each mixture circulating in the pipelines connected to each other, especially by near-infrared spectroscopy, and using a multivariable regression or god = network type. Iterative adjustment algorithm Method, which tends to reduce the difference between the actual value and the setting value of characteristics. The algorithm used here is the "black box" formula, which has the disadvantages of this method: considerable implementation time, because the result is only obtained after a number of tests, which can only be tested. It is used in the field and its 6 paper sizes are applicable to China National Standard (CNS) A4 specification (210X297 mm) f. Read the notes on the back before filling in this page. Policy,-* A7 B7 Central Bureau of Standards, Ministry of Economic Affairs Printed by the Consumer Cooperative Cooperative 5. Description of the invention (4 can only get very poor accuracy. In the following, the following words are marked:-bamboo shoot control variable: must be Ning from 4.zl 1 '"V fixed close to the pre Decide the set value of the set value, and it will display the process to the winter sigh, change the purity, separate the rare element pair-the rate of the given component, etc .; The operator changes the soil traverse, u ι number, such as flow • volume or allow to simulate the bed < replacement valve replacement period, etc.-access to j 彳 variables · Mainly acting on the area > Ran & '. ~: The 5 meaning variables in soap, such as acting on the part of the Buddha that is contained in β. + This is determined and transmitted to the operating variable. ^^ The number is the ¥ system algorithm. It needs to be reminded that the purpose of high-level private control intended to be used to separate the operation of the loop is to calculate a control law β benefit; then (all of the operating variables during the time ^ process), in order to: < *% J1: star 'ii g to calculate 4-able to produce Zhu _ or a number of control variables that have been selected in advance Two different control rules for the transfer of control, and adjustment operations, that is, to calculate-can _ all external control of the process disturbances as much as possible (or at least asymptotic) compensation, so that the previously selected control variables remain In the example of a simulated moving bed system, the disturbance caused by the thermodynamic and geometric parameters of the adsorbent (of course, the limited decline of the properties of the adsorbent) over time can also be compensated by adjustment. Some goals are achieved by an automatic control method intended to be used in the process of separating the components of the circulating fluid mixture according to the present invention, which can overcome the aforementioned disadvantages. It is not based on the " black box It is based on the more controlled paper size and applies the Chinese National Standard (CNS) A4 specification (210 × 297 mm) Ί.Γ -------- J 衣 -----— Order (谙 Please read the notes on the back before filling this page.) A7 __B7 printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the Invention (5)-The method of production is allowed by the non-linear mode of the separation method. Summary of Invention The method according to the present invention is applied to a simulated moving bed system (or unit) for separating components, which includes a closed loop consisting of tower beds connected in series with each other and containing adsorbent material. The fluid injection and extraction points are divided into several areas, the device for injecting fluid into the circuit, the device for taking fluid out of the circuit, the injection point and extraction point conversion device capable of reversely replacing the beam tower, and Device for measuring each variable (such as concentration, flow rate, valve switching period, etc.). It contains: ~-Measurement operation variables and the concentration of certain components, which are required to calculate the control variables at many points on a separation circuit at least equal to 2;-The measurement variables are lacking, and a separation is used The system (can be a non-linear mode, or a linear approach to a given operating point; ^) has determined the mode of operation to determine the respective labeled ratio 値 (Rk), which is in each different area, intermediary Between the fluid flow rate (QK) and the simulated adsorbent material flow rate, to bring the control variable to or back to the determined setting, and • From this ratio (Rk), determine the value of the desired operation variable. On a separation loop region containing an array of adjacent stages including the η region, η ratios 値 (Rk) are defined. This method usually includes the root flow rate (D) and the concentration 値 (X) to define the m-phase controlled variable (Ξ), where m 値 is less than or equal to η 値, measure (to the example of the non-linear control mode) the concentration (X) of the ~ end point in the liquid phase and determine m this ratio 値 (Rk ) Or the ratio of m to m, which contains (nm) parameters. A specific example of a separation circuit with four main areas, Example-8-1 Paper size ^ Use Chinese National Standard (CNS) A4 size (2ΐ〇χ29 · 7mm) '(Please read the precautions on the back before (Fill in this page) Λ 衣 · 、-° A7

經濟部中央標準局員工消費合作社印製 如迴路效率與混合物之至少一組份之純度之控制變數(ξ) 係同時從不同濃度之線上測量以控制。 例如係使用拉曼(Raman)式之線上分析、色層分析或近 紅外線(NIR)分析以用於濃度測量。 根據一具體實袍例,在具有四個g域之分離單元或系統 之例子中,係選擇下述四個量中之至少一個以作爲被控制 變數:從迴路所取出之流體中之第一组份之純度、分離系 統對一組份(與第一组份或其他者相同)之產率、該第一組 份在與流艟之循環方向有關之此四區之第一者^之後部之尾 量、及/或除了該第一组份外所有組份之尾量,其係在與 流體之猶環方向有關之此四區之最後者之前部。 在含有特定數目p之區域之分離系統中之已知比値(Rk) 之値下’本方法允許去決定由飼入至少—個額外之注入點 及/或至少一個取出點至分離迴路中所形成之額外比値之 對應値,其係根據鄰近區域之比値之已知値以及根據所考 慮之注入及/或取出流量。 在取出流體中之组份濃度間之比値之値可以選擇以作爲 被控制變數。 一最適化之演算法可以有利地使用。 所用之方法可以輕易地使用於控制許多之被控制變數 (ξ ) *只要其係比值(Rk)。這些被控制變數可以例如是產· 量、溶劑比例、尾量測量等》 根據本發明之方法能夠維持分離單元之穩定運作,即使 是在流量或進料品質改變存在下。 -9- ^紙張尺度適用中國國家標準(CNS ) A4規格(210><297公釐〉 ~—:- (錆先閱讀背齒之泣意事項蒋填寫本買) 装. A7 B7 經濟部中央標準局員工消費合作社印製 五、發明説明(7 ) 圖示簡要説明 從閲"讀下文非限制性之具體實施範例之描述、以及配合 參考所跗之圖示’根據本發明之其他特色與優點可以更清 楚: . -圖1爲眞實移動床分離迴路之流程, -圖2係辉明使用於材料平衡方程式之不連續性之原則, -圖3爲説明比値計算之迴路之二個區域間之區間之流程’ -圖4所示爲迴路控制方法之各相之流程圖, -圖5爲具肴四個區域之分離迴路之流程圖,四個注入或取 出點以及八個測量點, -圖6所7F爲進料組成改變之時間記錄,其係爲了在下述之 模擬中説明調整範例, 身· 4. 圖7所示爲由於改變飼入之結果,二個被控制變數進展之 時間記錄,即萃取物之純度與單元產率, -圖8所示爲在相同之條件下所提供之控制效率,其係藉施 用根據本發明之方法,且 -圖9至ί2所示爲當製程穩定時與四個操作變數有關之進展 時間記錄,其分別爲循環流量(圖9 )、萃取物流量(圖丨〇 ) 、變換期(圖11)與萃餘、物流量(圖12卜 發明詳述 一種含有封閉之分離迴路以及模擬移動床之分離單元,— 其係被至少分成四區,每一區與相鄰者藉注入或取出流以 刀隔’該注入與取出流本質上係在固定之時間.間隔下替換 。該迴路具有—用以循環該混合物之泵,其輸出係被控制 -10- 本紙張尺度通用宁國國家標率(CNS ) A4» (210X297公釐) (餚先閱讀背面之注意事項再填寫本頁) ----- ,爹------訂 A? B7 經濟部中央標準局員工消費合作社印製 五、發明说明( 士係放置於二個連續之塔柱或塔區間,以及可能至少一個 塔區間。.又i裝置,其亦攻置於二個連續之塔柱或 、一拉曼式之測量裝置可以有利地使用,其係例如申請人 所申請二法國專利第2,699,917號(A國專利第5,569,綱號 J 斤描述」其可以使用於大量之即時濃度洌量且因此能 于者迴路不同點處之濃度分怖。隨意地選擇n個明 g也刀佈於不同區之(對具有四區之分離系統,打通常範圍 在2 ” 8冬簡)測量係可充份地確保演算控制方法之平順運 作。 ' I)變數之選擇 a)被控制豢 被控制變數係定義爲數個變數之: (1) $ = F(D,X),其中 -X # —向量,代表在不同點處液相之各個組份之濃度(此 値可以.表即時的或在變換期所取値之平均)。 -D係一向量’其之每一個元素爲内部之注入或取出流量。 • I _ 在早元(例如在向外流)之任何點處液相之組份之純度ξ 可以作爲被控制變數之範例: ξ = χί/(χί+^ρ〇,Λ- t , -Xi爲在给定點處組份i之濃度。 -Impi爲在此點處被考慮爲雜質之其他組份之濃度和(其可 以排除某些組份例如洗脱劑)。 -11 - 本紙張尺度適用中國國家標隼(CMS ) A4規格(210X297公釐) (讀先閱讀背面之注意事項再填寫本頁) ^—«^1 TJ m nn ^^^^1 · •va. A7 B7 五、發明説明( 在給定之時間此被控制變數之計算,因此包含在迴路之 -或多個點處之液相t·所有存在濃度之測量。這些測量可 以例如藉上逑所提之拉曼式分析或藉任何其他之方 行。 該被控制變數可以事先自由地選#。友四區單元之例予 中,操作者*常使用以企求之量可以例如被選擇以作爲被 控制變數: 1) 萃取物之其中一組份之純度, 2) 單元對此組份之產率 - 3) 點〇與2)所考慮组份之尾量,在區i之後^(與流體之 循環方向有關), 4) 除了在點1)、2>或3)處所考慮之组份外、所有組份之 尾量,在區4之前部(與流體之循環有關)。 b)控制變數 拫據本發明之方法包括藉由欲给操作變數之値以選擇控 制變數,其係爲了使被控制變數之進展之控制可以被直接 決定^ 經濟部中央標準局員工消費合作社印製 ......... - - 11'-.1 - . 1--. I (諳先Μ讀背面之注意事項再填寫本頁) 廷些控制變數轉變成"傳统之"操作變數係總是可能超出 與製程以及設備之尺寸有關之眞實物理應用之限制,同爲 在其之間有一對一之關係,其係分離系統欲良好控制之必 須條件。 _ 在所有操作變數係自由(即這些値可以自由地固定,無 須考慮物理之限制)之例子中,獨立控制變數之必須數目' 係等於形成分離單元之區域數。 12- 本紙張尺度適用中國國家標準(CNS ) A4規格(2丨〇><297公釐) A7 B7 經濟部中央標準局員工消費合作社印掣 五、發明説明(10 模擬移動床分離系統之操作係準相同於眞實移動床系、、 者係熟知的,當後者若與主要液體流反向之循環流=係J 下述闕係給定時·· aPrinted by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs. For example, the control variable (ξ) of the loop efficiency and the purity of at least one component of the mixture is measured at the same time from different concentration lines for control. For example, Raman-type on-line analysis, color layer analysis, or near-infrared (NIR) analysis is used for concentration measurement. According to a specific example, in an example of a separation unit or system with four g domains, at least one of the following four quantities is selected as the controlled variable: the first group of fluids taken from the circuit The purity of the components, the yield of the separation system for one component (same as the first component or the others), the first component in the first four of the four areas related to the circulation direction of the flow. The tail amount, and / or the tail amount of all components except the first component, is in front of the last of the four zones related to the direction of the fluid. Under a known ratio (Rk) in a separation system containing a specific number of p's, this method allows the decision to feed from at least one additional injection point and / or at least one extraction point to the separation circuit. The corresponding 値 of the additional ratio 値 is based on the known 値 of the ratio 邻近 of the adjacent area and according to the injection and / or withdrawal flow considered. The ratio between the component concentrations in the removed fluid can be selected as the controlled variable. An optimization algorithm can be used to advantage. The method used can be easily used to control many controlled variables (ξ) * as long as it is the ratio (Rk). These controlled variables can be, for example, production · volume, solvent ratio, tail measurement, etc. The method according to the present invention can maintain stable operation of the separation unit, even in the presence of changes in flow rate or feed quality. -9- ^ Paper size applies Chinese National Standard (CNS) A4 specification (210 > < 297mm> ~~:-(锖 Please read the weeping matter of back teeth first and fill in this purchase) Pack. A7 B7 Central Ministry of Economic Affairs Printed by the Consumer Bureau of the Standards Bureau. 5. Description of the invention (7) A brief description of the diagram. From the "Read the following description of the non-limiting specific implementation examples, and with reference to the drawings" according to other features of the present invention and The advantages can be made clearer:-Figure 1 is the flow of the solid moving bed separation circuit,-Figure 2 is the principle of discontinuity used by Huiming for the material balance equation,-Figure 3 is the two areas illustrating the calculation of the ratio calculation The flow of the interval '-Figure 4 shows the flow chart of the phases of the loop control method,-Figure 5 is the flow chart of the separation circuit with four areas, four injection or extraction points, and eight measurement points, -7F in Fig. 6 is the time record of the feed composition change, which is used to illustrate the adjustment example in the following simulation. Figure 4 shows the time when the two controlled variables progress due to the result of changing the feeding. Record, purity of the extract Unit yield,-Fig. 8 shows the control efficiency provided under the same conditions by applying the method according to the present invention, and-Figs. 9 to 2 show that it is related to four operating variables when the process is stable The progress time records are respectively the circulation flow rate (Figure 9), extract flow rate (Figure 丨 0), conversion period (Figure 11), and raffinate and material flow rates (Figure 12). The invention details a closed separation circuit and The separation unit of the simulated moving bed, which is divided into at least four zones, and each zone is separated from the neighbor by injecting or extracting the stream. The injection and the extracting stream are essentially replaced at a fixed time interval. The The circuit has—the pump used to circulate the mixture, and its output is controlled-10- This paper size is Ningguo National Standard (CNS) A4 »(210X297 mm) (Please read the precautions on the back before filling this page ) -----, Dad ------ Order A? B7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. 5. Description of Invention (The scholarship is placed in two consecutive towers or tower sections, and may be at least A tower section .. and i device, which also attacked A continuous tower or a Raman-type measuring device can be advantageously used, which is, for example, applied by the applicant for two French patents No. 2,699,917 (country A patent No. 5,569, outline No. J). It can be used in a large number of The instant concentration and volume can be distributed at different points in the circuit of the user. Randomly select n bright g also be clothed in different zones (for a separation system with four zones, the usual range is 2 ”8 winter Jane) The measurement system can fully ensure the smooth operation of the calculation control method. 'I) Selection of variables a) Controlled and controlled variables are defined as one of several variables: (1) $ = F (D, X), Where -X # — vector, represents the concentration of each component of the liquid phase at different points (this can be. Table shows the average of the instantaneous or taken during the transformation period). -D is a vector 'where each element is the internal injection or extraction flow. • I _ The purity of the components in the liquid phase at any point in the early yuan (for example, outflow) can be used as an example of the controlled variable: ξ = χί / (χί + ^ ρ〇, Λ- t, -Xi is Concentration of component i at a given point. -Impi is the concentration of other components that are considered as impurities at this point (which can exclude certain components such as eluents). -11-This paper scale applies to China National Standard (CMS) A4 specification (210X297 mm) (Read the precautions on the back before filling this page) ^ — «^ 1 TJ m nn ^^^^ 1 · • va. A7 B7 V. Description of the invention ( The calculation of this controlled variable at a given time, and therefore includes measurements of the liquid phase t at the point or points of the circuit, all concentrations present. These measurements can be made, for example, by Raman-type analysis mentioned above or by any Others can be controlled. The controlled variable can be freely selected in advance. In the example of the friend four-zone unit, the operator * often uses the desired amount. For example, it can be selected as the controlled variable: 1) Among the extracts The purity of one component, 2) the yield of the component to this component-3) points 0 and 2) the end of the component under consideration After the zone i ^ (related to the circulation direction of the fluid), 4) Except for the components considered at points 1), 2 > or 3), the tails of all components are before the zone 4 (and Fluid circulation). b) Control variable: The method according to the present invention includes selecting a control variable by giving an operation variable, which is so that the control of the progress of the controlled variable can be directly determined. .........--11 '-. 1-. 1--. I (I read the precautions on the back and then fill out this page) These control variables are transformed into " traditional " operations Variables are always beyond the limits of solid physical applications related to the process and the size of the equipment. They also have a one-to-one relationship between them, which is a necessary condition for the separation system to be well controlled. _ In the example where all operating variables are free (that is, these 値 can be fixed freely without having to consider physical constraints), the necessary number of independent control variables' is equal to the number of regions forming the separation unit. 12- This paper size is in accordance with Chinese National Standard (CNS) A4 specification (2 丨 〇 < 297 mm) A7 B7 Printed by the Staff Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention (10 Simulated moving bed separation system The operation system is almost the same as that of the solid moving bed system, which is well-known. When the latter is opposite to the main liquid flow, the circulating flow is = J. The following is the given timing ... a

(2) Q s=( % V micro* Vcolumn) /T(2) Q s = (% V micro * Vcolumn) / T

Qs爲"固體流··(對應有效之容量),其係對等於在模擬移 床單元中閥變換所產生者。Qs is " solid flow ... (corresponding to the effective capacity), which is equal to the valve changer generated in the simulated moving bed unit.

(3) q e=( % V macro+ % V meso+ % V vi) * V column) / T qe爲”液體反向流”,其係對等於閥變換所產生者。其對應 於包含在中-與巨孔中以及在外部孔洞或加至^床孔洞^ 顆粒孔洞中之液體量。其通常被視爲"阻流”或載流。其^ 應於未袜吸附劑之微孔洞所吸附之液體之停滯性。 、’ 在(2)與(3)之關係中 i 11 -T爲模擬移動床單元之閥之變換期之値, -Vcolumn爲單元區域之基本體積(包含於二個連續注入及卜 取出點,間之體積’活化或否), 一 -%VmiaO、%Vmeso、%Vmacr〇、%Vv丨分別爲微孔(有效容量 、中孔、巨孔體輪以及塔床之外部孔洞之百分率。 ) 未出現在式(3)之靜滯體積且對應於連續篩床間之靜 體積,係經由整體地增加式(3)之各個百分率以考建。、 對此二個單元形式,其外部之液體流係相同的。在另―― 方面,模擬移動床與眞實移動床間之内部流動並不相同 這些流動藉下述之鬭係以關連:°(3) q e = (% V macro +% V meso +% V vi) * V column) / T qe is the "reverse flow of liquid", which is equal to the one generated by the valve transformation. It corresponds to the amount of liquid contained in the meso- and macropores as well as in the external holes or added to the bed holes ^ particle holes. It is usually regarded as " blocking current " or current carrying. It should be the stagnation of the liquid adsorbed by the micropores of the non-sock adsorbent., '' In the relationship between (2) and (3) i 11- T is the transition period of the valve of the simulated moving bed unit, -Vcolumn is the basic volume of the unit area (contained between two consecutive injection and extraction points, and the volume is 'activated or not'),-% VmiaO,% Vmeso ,% Vmacr0,% Vv 丨 are the micropores (effective volume, mesopores, megapore body wheels and the percentage of external holes in the tower bed.) The static volume that does not appear in formula (3) and corresponds to the continuous sieve bed The static volume is based on the overall increase of each percentage of formula (3). For these two unit forms, the external liquid flow is the same. In the other aspect, the simulated moving bed and the solid movement The internal flows between the beds are not the same. These flows are related by:

Qfc=Fk+qe -13 本纸張尺度適用中國國家標準(CNS ) A4規格(210 X 297公楚) ..—j_ - .. I 装 訂 (請先閱讀背面之注意項再填寫本頁} A7 B7 五、發明説明(H ). 其中Qk爲通過模擬移動床單元之區域^之液體流動,Qfc = Fk + qe -13 This paper size applies to Chinese National Standard (CNS) A4 (210 X 297 cm) .. —j_-.. I Binding (Please read the notes on the back before filling this page} A7 B7 V. Description of the invention (H). Where Qk is the liquid flow through the region ^ of the simulated moving bed unit,

Fk爲通過眞實移動床單元之區域k之液體流動。 若我們採用維持靜止之非吸附追蹤劑之範例,對眞實移 動床單元該必須流動爲0,但對過模擬移動床單元,其等 於阻流qe。 ~ 、 由這些定義,所選擇之獨立控制變數爲4無因次之比値 或比値Rk(k=〗,2,3或4),其係介於在每一區中之主要液體 流與在整個單元中爲定値之固體流間: (4) Rk=Qk/Qs 用於控制之4比値Rk之選擇係耒自眞實移動床單元之模 式之物質平衡方程式,其係在穩態下在不連續之塔柱分部 中。在考慮反向流體流動下,配合三點j, j + Ι)進行之 不連續.性係藉下述之範例以·表示。 藉指定在液相中於點j處組份i之濃度爲Xij且在點j處於 固相中此組份之平衡溧度爲yu ’(圏2)對此组份之物質平 衡係表步如.下: 經濟部中央標準局員工消費合作社印掣 —^n 4VH t^i^l ml m^l m n m n^i tf fm 一·、 - s. 、v-a (請先閲讀背面之注意事項再填寫本頁)Fk is the liquid flow through area k of the solid moving bed unit. If we use the example of a non-adsorbed tracker that remains stationary, it must flow to zero for a real moving bed unit, but it is equal to the flow restriction qe for an simulated moving bed unit. ~, From these definitions, the selected independent control variable is 4 dimensionless ratio 値 or ratio 値 Rk (k =〗, 2, 3 or 4), which is the main liquid flow in each zone and In the whole unit, the fixed solid flow is: (4) Rk = Qk / Qs 4 ratio for control. The selection of Rk is the material balance equation of the model of the solid moving bed unit, which is under steady state at Discontinued Tower Column Division. Considering the reverse fluid flow, the discontinuity performed with three points j, j + Ι). The property is represented by · by the following example. By specifying that the concentration of component i in the liquid phase at point j is Xij and the equilibrium degree of this component in the solid phase at point j is yu '(圏 2) The material balance for this component is as shown in the table. Bottom: Printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs— ^ n 4VH t ^ i ^ l ml m ^ lmnmn ^ i tf fm i.,-S., Va (Please read the precautions on the back before filling this page )

Qk(Xiij.rXij)+Qs(yij+i-yij)+tle(xy+rxi1i)=:〇 即藉除以Qs : (5) (Qfc/Qs)(Xij-i-xy)+ (yiJ+i-yij)+(qe/Qs)(Xij+rXij)=0 配合Qs與qe之個別定義,藉關係(1)、(2)表示: _ %Vmes〇 ++ κ =定儘 Qs %Vmicro 且式(5)係表示成下述: -14- 本纸張尺度適用中國國家標準(CNS ) A4規格(2丨公釐) 經濟部中央標準局員工消費合作社印製 A7 B7 五、發明説明(12 ) (7) Rk(xij.rxu)+(yy+1-yij)+K〇(xu+rxij)=0 唯一之控制變數(上述方程式之可自由修改之參數)爲比 値Rk,考慮其之定義,其在形成車元之每一區中係已知的 。比値之數目與區數相同。根據使用者或操作者之偏好, 這些比値可以轉變成通常之操作變數,其係與Qki値具有 非奇異代數關係。 在一 4-區之單元中,在4個比値與下述5個操作變數中之 4個具有一對一之關係: T, Ql, Qsolvent, Qextract, Qfeedstock 备- 該第五個變數爲需決定去卣定之參數(pamm)。其最通常爲 進料流量Qfeedstock。結果,得到下述比値與操作變數間之 關係: tQk (Xiij.rXij) + Qs (yij + i-yij) + tle (xy + rxi1i) =: 〇 That is, divide by Qs: (5) (Qfc / Qs) (Xij-i-xy) + (yiJ + i-yij) + (qe / Qs) (Xij + rXij) = 0 According to the individual definitions of Qs and qe, expressed by the relationship (1), (2): _% Vmes〇 ++ κ = Determine Qs% Vmicro and Formula (5) is expressed as follows: -14- This paper size is applicable to Chinese National Standard (CNS) A4 (2 丨 mm) A7 B7 printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention (12 ) (7) Rk (xij.rxu) + (yy + 1-yij) + K〇 (xu + rxij) = 0 The only control variable (the freely modifiable parameter of the above equation) is the ratio 値 Rk, consider it Definitions, which are known in each zone forming a car element. The number of ratios is the same as the number of zones. According to the user or operator's preference, these ratios can be transformed into ordinary operational variables, which have a non-singular algebraic relationship with Qki 値. In a 4-zone unit, there is a one-to-one relationship between the 4 ratios and 4 of the following 5 operating variables: T, Ql, Qsolvent, Qextract, Qfeedstock. The fifth variable is required. Decided to set the parameters (pamm). It is most often the feed flow Qfeedstock. As a result, the relationship between the following ratio 値 and the operating variable is obtained: t

•a»·. A 若 param= Qfeedstock T=% V micro* V column* (R3-R2) / param• a ».. A if param = Qfeedstock T =% V micro * V column * (R3-R2) / param

Ql=param*Rl/(R3-R2) 'Qsolvent=param*(Rl-R4)/(R3-R2)Ql = param * Rl / (R3-R2) 'Qsolvent = param * (Rl-R4) / (R3-R2)

Qextract=param*(Rl -R2)/(R3-R2) 此系統係定義,若param<>0(其係亦對等於R3<>R2)。 從5個中選出4個變數允許範例去運作:Qextract = param * (Rl -R2) / (R3-R2) This system is defined if param < > 0 (which is also equal to R3 < R2). Select 4 variables out of 5 to allow the example to work:

I '-配合固定或可變之進料,但其係藉製程以施加, -或配合一固定之溶劑流量, -配合固定之閥變換期,等。 II)比値計算演算法 1)非線性模式 -15- 本紙張尺度適用中國國家標隼(CNS ) A4規格(2丨0X297公釐) 11 -- · _ - - --- - - i t^i— —^m __ _ y , . · 穿. (請先閱讀背面之注意事項再填寫本頁)I '-with a fixed or variable feed, but it is applied by a process,-or with a fixed solvent flow,-with a fixed valve change period, and so on. II) Ratio calculation algorithm 1) Non-linear mode -15- This paper size is applicable to China National Standard (CNS) A4 specification (2 丨 0X297 mm) 11-· _-------it ^ i — — ^ M __ _ y,. · Wear. (Please read the precautions on the back before filling this page)

第87106265號專利申請案 中文說明書修正頁(88年11月、 五、發明説明(13) 該計算演算法包括真實移動床單元之非線性物理模式, 其能夠計算比值(如段II中所定義),所以被控制變數可以 在事先得到固定之值。該計算方法係費力、非t迅速且暗 示在線上足夠之測量是可以的。 a) 比值計算原則 ; 將由熟習該項技藝之人士所適當選擇之數目為m之式(〇 所給之形式之被控制變數限制於區段中,其中m係小於或 等於η ’即一組相鄰包括一或多個區域之階段,其中係定義 η偏比值。藉由定義統計模式之代數式以及在區段之端 點處之液相中之濃度之可得測量,這些m個被控制變數能 夠計算m個比值或含有(n-m)個參數之這些比值之m種合併 〇 b) 對4-區單元之純度計茸籁例 純度ξρ係只能從萃取物(Xert)之組成之認知中定出: gp = F(Xert) 選擇一包含區域1之部份以及區域2之部份之區段(圖3), 其中2個比值因此可定出。比值r 1、在端點處之液相中所 有组份之濃度Xe與Xs以及純度之設定值(被控制變數)之認 知能夠去計算比值R2。 實際上,從式(7)且對組份i (指數m表示真實之測量值), 我們可以窝出: -在階段e+1 :Revised page of Chinese Specification for Patent Application No. 87106265 (November 88, V. Description of Invention (13) The calculation algorithm includes a non-linear physical model of a real moving bed unit, which can calculate the ratio (as defined in paragraph II) Therefore, the controlled variable can get a fixed value in advance. The calculation method is laborious, not fast and implies that sufficient measurements are available online. A) The principle of ratio calculation; it will be appropriately selected by those skilled in the art The number of equations in the form of m (0 is limited to the controlled variables in the form of m, where m is less than or equal to η ′, that is, a group of adjacent stages including one or more regions, where η partial ratio is defined. By defining an algebraic expression of the statistical model and the available measurement of the concentration in the liquid phase at the endpoints of the segment, these m controlled variables can calculate m ratios or m of these ratios containing (nm) parameters Merging 〇b) The purity of the 4-zone unit is calculated. For example, the purity ξρ can only be determined from the knowledge of the composition of the extract (Xert): gp = F (Xert) Select a part that contains region 1 and The segment portion of domain 2 (FIG. 3), wherein the two ratios thus fix. The ratio r1. The knowledge of the concentration Xe and Xs of all components in the liquid phase at the endpoints and the knowledge of the setpoints (controlled variables) of purity can be used to calculate the ratio R2. In fact, from equation (7) and for component i (the index m represents the true measured value), we can find out:-at stage e + 1:

Ri(xmi,e-Xi,e+i) + (yi,e+ryi,e+i)+K(Xi,e+2-Xi,e+1)=0 -16- 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) 一請先閲讀背面之注意事項符填寫本寅〕 ,ίτ 經濟部中央標準局員工消費合作杜印裝 A7 A7 經濟部中央標準局員工消費合作社印製 B7 五、發明説明(14 ) -在包含於階段e與萃取物取出階段ext間之階段j : R1 ( X i j.r x i j)+(y i j+r y i.j)+K ( X i j+1- X i j)=0 -對應於萃取物取出之階段ext : R 1 ( X i,ext-l_ X ( y i,ext+l_ y i,ext) + K ( X i,bxt+]· X i,ext) = 〇 -在包含於萃取物取出階段ext與階段s-l間之階段k : R 2 ( X i,k-r X i,k)+(y i,k+r y i,k)+K ( x i,k+i-x i,k)=〇 -在階段卩-1 : R 2 (χ i,s-2- x i;s-i)+(y m i)S- y i,s-i)+κ (xm ijS- Xi.s.0=〇 ^ c)溶液之存左 考慮前述方程式之形式,若方程式之數目等於未知數之 數目,則會有單一解。該未知數爲Μ一個階段存在於液 相中之组份之濃度値加上區域2中之比値,即 + 1 ’其中nc表示組份之數目。 、=式之數目等於在…與⑴間包含之階段數乘以组份 2數二I?—.1)。一補充之方程式藉所欲之被控制 .丈數値以產生,即€P_F(xert)=〇。 此系統之尺寸之非線性代數方程式: Cnc(s~e+l)+l]*[nc(s-e+l)+i] 係藉牛頓趨近法以解答。其他之輪出函數 基. 量可以相似地定出。 ^產率、尾 某些其他明顯地與流章値有關 中。例如,分離單元之組份i之產率可:以加至單元 —-17- 適用 TiS 標準(;)A4 規格(210x297^~ --^- ---------. '^衣---n I I (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費合作社印製 A7 B7 五、發明説明(15 ) 產率=10 0 - (Q raP X M) / (Q feedstock* X 1/eedstock)。 此方程式可以簡單地表示成比値之函數: d) 範例 - 下述所呈現之模擬乃關於二申苯分離單元,其具有模擬 之移動床以及4個區'(在任付方面上都非限制本發明應用之 範圍)。吾人企圖去純化從萃取物中取得之對二甲苯。該 進料含有5種组份:對二甲苯、__二甲苯、鄰二曱苯、乙 苯與萃餘物。二個主要被控制變數爲對二甲苯1屯度與分離 單元之對二甲苯產率。被控制變數之値與在芳香族加工迴 路中分離單元之位置有關。 該分析設備必須在精確度與反應時_上適合欲測量之輸 出函數。 e) 被控制變數之選擇: 1) 在萃取物中對二甲苯之純度藉下述之關係以定出: 41=P.5Ce/(PXe+IMPe),其中 -PXe爲在萃取物取出點之液相中對二甲苯濃度之平均値, -IMPe爲存在於遠離溶劑(以及可能爲萃餘物)之萃取物取 出點液面處之液相中之其他組份之濃度和。 ξ 1之値主要與IMPe値有關,因爲PXe本質上爲定値。 IMPe主要與區域2中之比値(R2)有關。 2) 單元之對二甲苯產率藉下述之關係以定出: -18 - 本紙張尺度適用中國國家標隼(CNS ) A4規格(210X297公釐) ^ - 裝 . 訂 (讀先Μ讀背面之注意事項再填寫本頁) 五、發明説明(16 ξ2 PXeQextract A7 B7 PXcQfeedstock + PXsQsolvent 或其在穩態時之同等式: PXcQfeedstock + PXsQsolvent — PXiQraffmate ξ2 PXcQfeedstock + PXsQsolvent 經濟部中央標準局員工消費合作社印f 其中PXc、PXs與PXr分別爲在進.料、溶劑與萃餘物之液相 中對二甲苯之濃度値。 Q extract、Q feedstock、Q solvent 與 Q faffinate 分別爲卒取物、進料、落劑 與萃餘,物之流量。 _ ξ2之値主要與PXr之値有關,因此與區3之*比値(R3)有 關。其亦與進料、溶劑與萃餘物之流量以及進料與溶劑中 之對二甲苯組成有關。 考慮先前關於含有四區之單元之可·用控制變數之解釋, 必須選擇二個額外之被控制變數。 3) 在區1之後方(關於流體之循環方向)處之液相中對二 甲苯之尾量,其可以藉下述之關係以定出: ξ3=ΡΧ4 所選擇之測量點係位於區4長度之3/4處。ξ3之値主要與 區1之比値(R1)有關。 4) 在區4之前方(關於锍體之循環方向)處除了對二甲苯 外所有組份之尾量,其可以藉下述之關係片定出: ' ξ4=ΙΜΡΙ 其中ΙΜΡΙ爲除了對二甲苯與溶劑(且可能是萃餘物)外, 存在於液相中之所有組份之濃度和。 19- 本紙張尺度適用中國國家標準(CNS ) A4規格(2l〇X297公釐) (請先閱讀背面之注意事項再填寫本頁) -哀 、-° 經濟部中央標隼局員工消费合作社印製 Α7 Β7 五、發明説明(17 ) 所選擇之測量點係位於區1長度之1/4處。ξ4之値主要與 區4之比値(R4)有關。 f) 控制演算法之實施:控制變數或比値計| 該控制原則包括在單元區段上模式方程式之使用。在所 選擇之例子中,係使用下述之三個^段: -第一區段T1係包含於區4之中部與區1之中部間。其能夠 同時計算區4 (R4)與區i (R1)中之比値。此係可能的,因爲 被控制變數ξ3與ξ4係於此區段中定出。 -第二區段係包含於區1之中部與區2之中部間。此區段 在R1已知下,能夠計算比値R2。變數以係位於此區段之 _中部。 -第三區段T3係包含於區3之中部與區4之中部間。此區段 在R4已知下,能夠計算比値r3。^·數、3係位於此區段之 中部七 從一實際之觀點,選擇單元中眞正可得到之操作變數係 在往後明智的。係選擇下述之玛侗變數:萃取物流、循環 流、洗Ιέ劑流與閥變換期丁(因此進料流被操作者選擇且萃 餘物流在所有時間可藉質量平衡以推算出)。對所考慮之 範例’在此單元上演算法之迴路係示於圖4中。 g) 模擬 從對分離單元之知識模式進行一模擬。此模式包括熱力_ •學,之知識以及動力學類之知識。此系統乏熱力學係藉吸 附等溫線以代表。在此處所探考之例子中,這些等溫線係 非線性立偶合。其可以爲η -組份通式化之藍穆爾 _ -20- 本,..氏浪尺反通用中國國家樣隼(CNS > Α4規格(2丨0'〆29"?公釐 (諳先閱讀背面之注意事項再填寫本頁}Ri (xmi, e-Xi, e + i) + (yi, e + ryi, e + i) + K (Xi, e + 2-Xi, e + 1) = 0 -16- This paper size applies to China Standard (CNS) A4 specification (210X297 mm) First, please read the note on the back to fill in the original text], ίτ The consumer cooperation of the Central Standards Bureau of the Ministry of Economic Affairs Du printed A7 A7 Printed by the Consumers Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs V. Description of the invention (14)-The stage j included between stage e and extract extraction stage ext: R1 (X i jr xij) + (yi j + ry ij) + K (X i j + 1- X ij ) = 0-Corresponds to the stage of extracting ext: R 1 (X i, ext-l_ X (yi, ext + l_ yi, ext) + K (X i, bxt +) · X i, ext) = 〇- In the phase k included between the extract extraction phase ext and the phase sl: R 2 (X i, kr X i, k) + (yi, k + ryi, k) + K (xi, k + ix i, k) = 〇- In phase 卩 -1: R 2 (χ i, s-2- xi; si) + (ymi) S- yi, si) + κ (xm ijS- Xi.s.0 = 〇 ^ c) solution Considering the form of the aforementioned equation, if the number of equations is equal to the number of unknowns, there will be a single solution. The unknown is the concentration of the components present in the liquid phase at one stage of M plus the ratio in region 2 (i.e., + 1 ') where nc represents the number of components. The number of, = formulas is equal to the number of stages contained between ... and 乘 times the component 2 (two I? —. 1). A supplementary equation is controlled by the desired. Counting to produce, that is, P_F (xert) = 0. The nonlinear algebraic equation of the size of this system: Cnc (s ~ e + l) + l] * [nc (s-e + l) + i] is solved by Newton's approach. The other round-out functions can be determined similarly. ^ Yield, tail Some others are obviously related to Liu Zhangyu. For example, the yield of component i of the separation unit can be: added to the unit—-17- applicable to the TiS standard (;) A4 size (210x297 ^ ~-^----------. '^ 衣--- n II (Please read the notes on the back before filling out this page) Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 V. Invention Description (15) Yield = 10 0-(Q raP XM) / ( Q feedstock * X 1 / eedstock). This equation can be simply expressed as a function of ratio 値: d) Example-The simulation presented below is for a Benzene separation unit with a simulated moving bed and 4 zones' (In terms of any payment, it does not limit the scope of application of the present invention). I tried to purify the para-xylene obtained from the extract. The feed contains 5 components: para-xylene, _-xylene, o-xylene, ethylbenzene and raffinate. The two main controlled variables are the paraxylene 1 degree and the paraxylene yield of the separation unit. The magnitude of the controlled variable is related to the position of the separation unit in the aromatic processing circuit. The analytical equipment must be suitable for the output function to be measured in accuracy and response time. e) Selection of controlled variables: 1) The purity of para-xylene in the extract can be determined by the following relationship: 41 = P.5Ce / (PXe + IMPe), where -PXe is at the extraction point of the extract The average p-xylene concentration in the liquid phase, -IMPe is the sum of the concentrations of other components in the liquid phase present at the level of the extraction point of the extract that is far from the solvent (and possibly the raffinate). The 値 of ξ 1 is mainly related to IMPe 値, because PXe is essentially fixed. IMPe is mainly related to the ratio 値 (R2) in region 2. 2) The p-xylene yield of the unit is determined by the following relationship: -18-This paper size applies to China National Standard (CNS) A4 specification (210X297 mm) ^-Packing. Please pay attention to this page before filling in this page) 5. Description of the invention Among them, PXc, PXs and PXr are the concentrations of para-xylene in the liquid phase of the feed, solvent and raffinate respectively. Q extract, Q feedstock, Q solvent and Q faffinate are stroke extract, feed, drop The flow rate of the agent and the raffinate and the material. _ The 値 of ξ2 is mainly related to the 値 of PXr, so it is related to the ratio * of the zone 3 (R3). It is also related to the flow of the feed, the solvent and the raffinate, and the feed and The paraxylene composition in the solvent is related. Considering the previous explanation of the available control variables for units containing four zones, two additional controlled variables must be selected. 3) Behind zone 1 (about the circulation of fluids) The tail amount of para-xylene in the liquid phase at the ring direction) can be determined by the following relationship: ξ3 = Ρχ4 The selected measurement point is located at 3/4 of the length of zone 4. The 値 of ξ3 is mainly related to the ratio 値 (R1) of zone 1. 4) The tails of all components except para-xylene at the front of area 4 (about the circulation direction of the carcass) can be determined by the following relationship sheet: 'ξ4 = ΙΜΡΙ where ΙΡΙ is except para-xylene Concentrations of all components present in the liquid phase with the solvent (and possibly the raffinate). 19- This paper size is in accordance with Chinese National Standard (CNS) A4 specification (210 × 297 mm) (Please read the precautions on the back before filling out this page) -Ai,-° Printed by the Consumer Cooperative of the Central Bureau of Standards, Ministry of Economic Affairs Α7 Β7 5. Description of the invention (17) The selected measurement point is located at 1/4 of the length of zone 1. The 値 of ξ4 is mainly related to the ratio 値 (R4) of zone 4. f) Implementation of control algorithms: control variables or ratios | This control principle includes the use of model equations on unit sections. In the selected example, the following three ^ segments are used:-The first segment T1 is included between the middle of the region 4 and the middle of the region 1. It can calculate the ratio 値 in zone 4 (R4) and zone i (R1) simultaneously. This system is possible because the controlled variables ξ3 and ξ4 are determined in this section. -The second section is contained between the middle of zone 1 and the middle of zone 2. With this segment known, the ratio 値 R2 can be calculated. The variable is located in the _center of this section. -The third section T3 is included between the middle of zone 3 and the middle of zone 4. This segment can calculate the ratio 値 r3 with R4 known. ^ · Number, 3 is located in the middle of this section. From a practical point of view, the operating variables that can be obtained in the selection unit are wise in the future. The following variables are selected: extraction stream, circulating stream, detergent stream and valve change period (so the feed stream is selected by the operator and the residual stream can be deduced by mass balance at all times). The circuit of the algorithm considered for this example 'is shown in Figure 4. g) Simulation Perform a simulation from the knowledge model of the separation unit. This mode includes the knowledge of heat, learning, and dynamics. The thermodynamics of this system is represented by adsorption isotherms. In the example examined here, these isotherms are nonlinearly coupled. It can be η-component generalized blue moor _ -20- this, .. the wave ruler anti-common Chinese national sample (CNS > Α4 specifications (2 丨 0'〆29 "? mm (谙Read the notes on the back before filling out this page}

五、發明説明( 18 A7 B7 經濟部中央標準局貝工消費合作社印製 Ϊ=1Γ)等,固定…選擇性)或較佳爲具有非固 定選擇性〈等溫線,例如具有藉一斜線連接之二個極限之 選擇性,或η-組份通式化之藍㈣_富_英德利奇 aangmUir-Freund„ch)等溫線。此系統之動力學係藉理論 板或藉指定至η個组份之每一侗之分*散係數以代表。 所使用之測量點數目爲8,其係如圖5中所分体。在此例 =中所使用之知識模式爲藍穆爾_富羅英德利奇等溫線配 S理論板之串級。測量之叙目以及其之位置係與區段之選 擇有關,其已如上所述地選擇;當然’此選擇在此處只是 用以説明且本發明函蓋與所需之目標相容之所^有區段之合 併。 口 所呈現〈結果係-控制之範例。該方法係以純度⑼ 與產率(95%)之固定設定値作用’以進科之组成係實質 上改變。纟+分鐘之穩定操作後(圖6),產±進料品質之 改變。 對進料,某一組份之體積叙成如下: ' 丁 〇1 = 0,022 Ρχ = 0.290 MxOx = 0.598 EB 0.102 Par = 0.032 一 某一進料之體積组成如下: T 〇1 = 0.024 P X = 0.290 先 閱 讀 背 '意 事 項 再 4 v ) 5..装V. Description of the invention (18 A7 B7 printed by the Central Standards Bureau of the Ministry of Economic Affairs, Printed by the Shellfish Consumer Cooperative, Ϊ = 1Γ), etc., fixed ... optional) or preferably non-fixed selective <isotherm, for example, connected by a slash The selectivity of the two extremes, or the blue isomerized by the general formula of η-component _ 富 _ 英 德利奇 aangmUir-Freund „ch) isotherm. The dynamics of this system is specified by the theoretical board or by η The fraction of each component of each component is represented by the dispersion coefficient. The number of measurement points used is 8, which is as shown in Figure 5. In this example, the knowledge model used in this example is Blue Moore_Fu Roying Derich isotherm with cascade of S theory board. The description of the measurement and its position are related to the selection of the section, which has been selected as described above; of course, 'this selection is here only for illustration and The present invention covers the merging of all sections compatible with the desired target. Oral presentation <Results-an example of control. This method is based on a fixed setting of purity ⑼ and yield (95%) '' The composition of Jinke has changed substantially. After a stable operation of 纟 + minutes (Figure 6), For the feed, the volume of a component is described as follows: 'Ding 〇1 = 0,022 Ρχ = 0.290 MxOx = 0.598 EB 0.102 Par = 0.032 A volume composition of a certain feed is as follows: T 〇1 = 0.024 PX = 0.290 first read the back of the matter and then 4 v) 5.

I 1 丁 -21 本紙張尺度適用中國國家標準(CMS ) A4规格(2丨〇X297公釐) 五、發明説明(19 ΜχΟχ ΕΒ Par a.512 0.190 0.032 ΑΊ Β7 經濟部中央標準局員工消費合作社印製 在圖5中所描述之擾動,於缺乏控制演|法、 „ 升古下疋效果係 示於圖7中。其係轉變成K2%之純i減少以及4〇/之產率厂 少。此製程因此對此進料品質之擾動係高度敏感 ' 將該相同之擾動施加至根據本發明之製程(圖 之穩定係進行約180分鐘,即3小時。純度之差異 ’最大之產率差異係低於〇.45%。可以注意的二R 思的*是四個控制 同時顯著地展開(圖9至12)。 在擾動之存在下,分離迴路之操作係難以藉操作員.以控 制’因其如前述所提必須同時作動四個變數。在此條件下 ’對高度熟練之操作員’其最快仍备花費24 ·〗、時以及數個 連續之穩定操作以期望去穩定該製程。 對穩定所必須之偏離規格暫時生產期上之明顯減小,其 藉實施根據本發明之方法所允許者,在工業上係轉變成相 闕生產力之增加。 h)變形: 爲了置放所有之操作變數,該演算法亦可以與本方法之 數値模擬模式聯合使用。 此處之目的係在許多例子:單元之定尺度、單元起始中, 使單元模式之運作最適化,使最後之最適化接近一已正確 鮮,使用具有不同分離間題之預存在單元等。當然,此麵 使用只能就模式而言視爲接近如前文中所提之物理眞實性 8 )。製程 並不顯著 _ M J--.---'J裝-- (諳先閲讀背面之注意事項再填寫本頁} ,1ΤI 1 Ding-21 This paper size applies the Chinese National Standard (CMS) A4 specification (2 丨 〇297297 mm) 5. Description of the invention (19 ΜχΟχ ΕΒ Par a.512 0.190 0.032 ΑΊ Β7 Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs The disturbance described in Fig. 5 is shown in Fig. 7 due to the lack of control method. The effect of Ascendant is shown in Fig. 7. It is converted to a reduction in pure i of K2% and a yield of 40%. This process is therefore highly sensitive to disturbances in the quality of this feed. 'The same disturbance is applied to the process according to the invention (the stability of the figure is carried out for about 180 minutes, i.e. 3 hours. The difference in purity is the' largest yield difference ' It is less than 0.45%. It can be noticed that the two R's * are the four controls that are significantly deployed at the same time (Figures 9 to 12). In the presence of disturbance, it is difficult for the operation of the separation circuit to be borrowed by the operator. As mentioned above, it must operate four variables at the same time. Under this condition, 'for highly skilled operators', the fastest can still spend 24 hours, hours and several consecutive stable operations in order to stabilize the process. Deviating from the specifications necessary for stability The significant reduction in the production period, which is implemented in the industry according to the method of the present invention, is transformed into an increase in relative productivity. H) Deformation: In order to place all operational variables, the algorithm can also be used with The numerical simulation mode of this method is used in combination. The purpose here is in many examples: unit scale, unit start, to optimize the operation of the unit mode, so that the final optimization is close to one that is already correct. Pre-existing units, etc. of different separation problems. Of course, this use can only be considered as close to the physical solidity as mentioned in the previous section 8). The process is not significant_ M J --.--- ' J Pack-(谙 Read the precautions on the back before filling this page}, 1Τ

J -22- 本纸張尺度適用中國國家標準(CNS) 格(210X297公釐) A7 .經濟部中央標準局員工消費合作社印製 五、發明説明(2〇 ) 。在此例子中,當然該調整値無法剛好產生所預期之性能 ’根據模擬模式之準確性,其可能較所欲者爲較低或較高 。演算法之迴路然後將能夠精確地從這些接近値達到該規 格〇 2&gt;線性模式 ·* 根據第二次之實施,從測量變數之眞實値來之比値 j決定可以藉使用單變數(輸出行爲之表示與輪入之變異 有關)或多變數(數個輸出行爲之表示與數個輸入有關)線 性模式以進行。這些&quot;簡單&quot;模式之決定係從一组配合在接 近預期之穩定狀態下運作&lt;製程所得之實驗測;^以進行。 這些模式通常係只代表接近系統之穩定工作點。 可以輕易地從這些模式合成—傳統之線性控制法射(内 部-模式控制 '預測控制式等)。該^之簡單性能夠輕易 地计算簡單與費力之控制法則,以補償所選擇表示之不精 確性。在模擬上,所計算之控制法則之性能測試係對應於 由製程之非線性物理模式所計算之控制法則所得者。 III)f施之豢基 1)額外之注入點 如前所述,存在於4-區單元例子中非線性與線性控制之 使用,可以絕對地施加至藉加入—或多個流體注入點所產 生之含有較多數目區域之分離單元中。在此例子中,比値— Rl、R2 ' R3與R4之計算仍維持相同,即使考慮到額外之 注入流已藉操作者加入(例如以進料或萃取物流之比例直 接或間接)。該比値之値與從已知鄭近比値以及所考慮之 -23 - 枣紙張尺度適用中1國家標準(CNS〉A4規格(210X297公羞〉 ^nn ^^^^1 ^^—^1 I.....—HI— I --- - 1·tm nn a _ i · 5 Γ諳先閔讀背面之注意事項再填寫本頁)J -22- This paper size applies to the Chinese National Standard (CNS) (210X297 mm) A7. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention (20). In this example, of course, the adjustment 値 cannot just produce the expected performance ′ Depending on the accuracy of the simulation mode, it may be lower or higher than the desired one. The loop of the algorithm will then be able to accurately reach the specification from these close 22> linear mode. * According to the second implementation, the ratio of 眞 to 眞, which is the actual value of the measured variable, determines whether a single variable can be borrowed (output behavior The representation is related to the variation of rotation) or the multivariate (the representation of several output behaviors is related to several inputs) linear mode to perform. These "simple" mode decisions are made from a set of experimental tests that work in conjunction with a process that is operating in a stable state close to the expected one. These modes usually represent only stable operating points close to the system. It can be easily synthesized from these modes—the traditional linear control method (internal-mode control, predictive control, etc.). The simplicity of this square can easily calculate simple and laborious control laws to compensate for the inaccuracy of the chosen representation. In simulation, the performance test of the calculated control law corresponds to the result of the control law calculated by the non-linear physical mode of the process. III) f Shi Zhiji 1) Additional injection points As mentioned above, the use of non-linear and linear control in the 4-zone unit example can be absolutely applied to the borrowed or generated by multiple fluid injection points In a separate unit containing a larger number of regions. In this example, the calculations for 値 —Rl, R2, R3, and R4 remain the same, even if it takes into account that additional injection streams have been added by the operator (eg, directly or indirectly in the proportion of the feed or extract stream). The ratio of this ratio is from the known Zheng Jin ratio and the -23-jujube paper size applicable to the national standard (CNS> A4 specification (210X297 public shame) ^ nn ^^^^ 1 ^^ — ^ 1 I .....— HI— I ----1 · tm nn a _ i · 5 Γ 谙 Read the notes on the back before filling in this page)

*1T 經濟部中央標牟局員工消費合作社印製 A7 B7 五、發明説明(21 ) 法入流量値所簡單產生之新注入有關。 2) 額外之取出點 如延伸1)中所述,存在於4-區單元例子中非線性與線性 控制之使用,可以施加至藉加入一或多個流體取出點所產 生之含有較多數目區域之分離單元+。在此例子中,比値 R2或R3之計算係根據新注入點所產生之額外比値來產生 。因此對每一個流體取出必須定出其輸出函數爲所欲規格 (例如純度或產率規格)之鬲數。在此例子中,對製程而言 每一個加入之取出流量値成爲新的獨立操作變數。 若考額外之取出沒有所欲之規格,則流動之値係藉操作 者以加入且我們係在與延伸2)相同之情況。 3) 额外之注入與取出點 如前所述,存在於4-區單元例子f/卩線性與線性控制之 使甩,可以施加至藉加入一或多個流體注入點以及一或多 個流體取出點所產生之含有較多數目區域之分離單禾中。 在前述二段文章中所描述之主張可以重複且全面化。 今)可選用之被控制變數 不論所選出之控制模式爲4個?丨述之被控制變數:成份 之純度、成份之產率(相同於純度或其他)以及在區1與區4 中之尾量値之非線性或線性者,其可以用新的被控制變數 取代,其係取出流體組成間之比値。例如,在萃取物中可一 以選擇同時控制對二甲苯之純度(主要係R2)以及由乙苯濃 度與間—甲苯和鄰二甲苯濃度和之比俊所定出之變數。該 後面之變數將主要受以之影響。 -24- 本纸張尺度適用中國國家操準(CNS) A4規格(2丨οχ”7公釐) —_ h―, . I 装 ^ 訂 (請先閏讀背面之注意事項再填寫本頁) A7 B7 五、發明説明(22 ) 5)控制模式之最適化 前述所定之非線性與線性控制可以與最適化演算法接合 ,其可以提出一系列用於延伸5)所描述被控制變數之設定 値,所以在減少由操作限制所定出之函數上,能夠保證最 適之操作。 _ , 裝 訂 (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製 -25- 本紙張尺度適用中國國家標準(CNS ) A4規格(210X 297公釐〉* 1T Printed by the Central Consumer Bureau of the Ministry of Economic Affairs, Consumer Cooperatives A7 B7 V. Description of the Invention (21) The new injection simply generated by the law's inflow rate is related. 2) Additional extraction points, as described in extension 1), exist in the use of non-linear and linear control in the 4-zone unit example, which can be applied to a larger number of areas generated by adding one or more fluid extraction points The separation unit +. In this example, the ratio 値 R2 or R3 is calculated based on the additional ratio 产生 generated by the new injection point. Therefore, for each fluid withdrawn, the output function must be set to the desired number (such as purity or yield specifications). In this example, for each process, the added extraction flow rate becomes a new independent operating variable. If there is no required specification for the extra take-out, then the flow is borrowed by the operator to join and we are in the same situation as the extension 2). 3) Additional injection and extraction points, as mentioned above, exist in the 4-zone unit example f / 卩 linear and linear control, which can be applied by adding one or more fluid injection points and one or more fluid extraction Dots produced by the isolated monograms containing a larger number of regions. The claims described in the two previous paragraphs can be repeated and comprehensive. Today) Can be used as the controlled variable No matter the selected control mode is 4?丨 The controlled variable described above: the purity of the component, the yield of the component (same as purity or other), and the non-linearity or linearity of the tail volume 区 in zone 1 and zone 4, which can be replaced by a new controlled variable , Which is the ratio 取出 between the components of the fluid. For example, in the extract, one can choose to control the purity of para-xylene (mainly R2) and the variable determined by the ratio of the concentration of ethylbenzene and the concentration of m-toluene and o-xylene. The latter variables will be mainly affected by it. -24- This paper size applies to China National Standards (CNS) A4 (2 丨 οχ ”7mm) —_ h―,. I Binding ^ (Please read the precautions on the back before filling this page) A7 B7 V. Description of the invention (22) 5) Optimization of control mode The aforementioned nonlinear and linear control can be combined with the optimization algorithm, which can propose a series of settings for extending the controlled variable described in 5) 値Therefore, in reducing the function determined by the operation limit, the optimal operation can be ensured. _, Binding (Please read the precautions on the back before filling this page) Printed by the Central Consumers Bureau of the Ministry of Economic Affairs and Consumer Cooperatives -25- This paper Applicable to China National Standard (CNS) A4 (210X 297mm)

Claims (1)

六、申請專利範圍 第87106265號專利申請 中文申請專利範圍修正太Scope of Patent Application No. 87106265 Patent Application 1 . 一種用於具有模擬移動床之組份分離系統控制之方去, 其包括一由互相串聯連接且含有吸附劑材料之塔床所組 成之閉分離迴路、其係藉流體注入與萃取點劃分成數2 區域、將流體注入迴路之裝置、將流體從迴路中取出之 裝置、旎夠模擬塔床之反向排代之注入點與取出點變換 裝置、以及測量操作變數之裝置,其特色為包含:又 -在沿著迴路之數個點上測量流體注入與取出特有之變 數以及運作該分離系統特有之變數, Λ -從測量變數之真實值且藉使用一分離系統之非線性模 式以決定各別標示比值之比值(Rk),其係在每—個不同 之區域中’介於流體流量(QK)與模擬吸附劑材料流量 (Qs)間,以將控制變數(ξ)帶至或帶回已決定之設定=, 以及 -從迠些比值(Rk)決定欲給至操作變數之值。 2 .根據申請專利範圍第1項之方法,其中該給定操作變數 之值係使用分離系統之非線性模式以決定。 3 .根據申請專利範圍第1項之方法,其中該給定操作變數 經濟部中央標準局員工消費合作社印製 • — J ^-- (請先閲讀背面之注意事項再填寫本頁y *1T 之值係使用接近給定運作點之分離系統之線性模式以決 定。 4.根據申請專利範圍第1或3項之方法,其中,在含有包括 η區且鄰接之階段之陣列之該分離迴路區域上,其中定 義出η個比值(Rk),包含根據流量值(D)與濃度值(X)定 義出m個被控制變數(ξ),其爪值係小於或等於11值,且 決定m該比值(Rk)或該比值之m合併,其含有(n_m)個參 本紙張尺度適用中國國家標準(CNS ) A4規格(210χ297公度) 六、申請專利範圍 第87106265號專利申請 中文申請專利範圍修正太1. A method for controlling a component separation system having a simulated moving bed, comprising a closed separation circuit composed of column beds connected in series with each other and containing an adsorbent material, which is divided by fluid injection and extraction points There are 2 areas, a device for injecting fluid into the circuit, a device for taking fluid out of the circuit, an injection point and take-out point conversion device sufficient to simulate the reverse replacement of the tower bed, and a device for measuring operating variables. : Again-measuring the unique variables of fluid injection and extraction at several points along the circuit and operating the unique variables of the separation system, Λ-from measuring the true value of the variables and using a non-linear mode of the separation system to determine each Do not indicate the ratio of the ratio (Rk), which is in each different area 'between the fluid flow rate (QK) and the simulated adsorbent material flow rate (Qs) to bring the control variable (ξ) to or back Determined settings =, and-From some ratios (Rk) determine the value to be given to the operating variable. 2. The method according to item 1 of the patent application scope, wherein the value of the given operating variable is determined using a non-linear mode of the separation system. 3. The method according to item 1 of the scope of patent application, where the given operating variable is printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs • — J ^-(Please read the precautions on the back before filling in this page y * 1T The value is determined using the linear mode of the separation system close to a given operating point. 4. The method according to item 1 or 3 of the scope of the patent application, wherein on the separation loop area containing an array of adjacent stages including the η region , Where η ratios (Rk) are defined, including m controlled variables (ξ) defined according to the flow value (D) and concentration value (X), whose claw value is less than or equal to 11 and determines the m (Rk) or the m combination of the ratio, which contains (n_m) reference paper sizes. Applicable to China National Standard (CNS) A4 specifications (210 x 297 degrees). 6. Patent application scope No. 87106265 Patent application Chinese application patent scope amendment too 1 . 一種用於具有模擬移動床之組份分離系統控制之方去, 其包括一由互相串聯連接且含有吸附劑材料之塔床所組 成之閉分離迴路、其係藉流體注入與萃取點劃分成數2 區域、將流體注入迴路之裝置、將流體從迴路中取出之 裝置、旎夠模擬塔床之反向排代之注入點與取出點變換 裝置、以及測量操作變數之裝置,其特色為包含:又 -在沿著迴路之數個點上測量流體注入與取出特有之變 數以及運作該分離系統特有之變數, Λ -從測量變數之真實值且藉使用一分離系統之非線性模 式以決定各別標示比值之比值(Rk),其係在每—個不同 之區域中’介於流體流量(QK)與模擬吸附劑材料流量 (Qs)間,以將控制變數(ξ)帶至或帶回已決定之設定=, 以及 -從迠些比值(Rk)決定欲給至操作變數之值。 2 .根據申請專利範圍第1項之方法,其中該給定操作變數 之值係使用分離系統之非線性模式以決定。 3 .根據申請專利範圍第1項之方法,其中該給定操作變數 經濟部中央標準局員工消費合作社印製 • — J ^-- (請先閲讀背面之注意事項再填寫本頁y *1T 之值係使用接近給定運作點之分離系統之線性模式以決 定。 4.根據申請專利範圍第1或3項之方法,其中,在含有包括 η區且鄰接之階段之陣列之該分離迴路區域上,其中定 義出η個比值(Rk),包含根據流量值(D)與濃度值(X)定 義出m個被控制變數(ξ),其爪值係小於或等於11值,且 決定m該比值(Rk)或該比值之m合併,其含有(n_m)個參 本紙張尺度適用中國國家標準(CNS ) A4規格(210χ297公度)1. A method for controlling a component separation system having a simulated moving bed, comprising a closed separation circuit composed of column beds connected in series with each other and containing an adsorbent material, which is divided by fluid injection and extraction points There are 2 areas, a device for injecting fluid into the circuit, a device for taking fluid out of the circuit, an injection point and take-out point conversion device sufficient to simulate the reverse replacement of the tower bed, and a device for measuring operating variables. : Again-measuring the unique variables of fluid injection and extraction at several points along the circuit and operating the unique variables of the separation system, Λ-from measuring the true value of the variables and using a non-linear mode of the separation system to determine each Do not indicate the ratio of the ratio (Rk), which is in each different area 'between the fluid flow rate (QK) and the simulated adsorbent material flow rate (Qs) to bring the control variable (ξ) to or back Determined settings =, and-From some ratios (Rk) determine the value to be given to the operating variable. 2. The method according to item 1 of the patent application scope, wherein the value of the given operating variable is determined using a non-linear mode of the separation system. 3. The method according to item 1 of the scope of patent application, where the given operating variable is printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs • — J ^-(Please read the precautions on the back before filling in this page y * 1T The value is determined using the linear mode of the separation system close to a given operating point. 4. The method according to item 1 or 3 of the scope of the patent application, wherein on the separation loop area containing an array of adjacent stages including the η region , Where η ratios (Rk) are defined, including m controlled variables (ξ) defined according to the flow value (D) and concentration value (X), whose claw value is less than or equal to 11 and determines the m (Rk) or the m combination of the ratio, which contains (n_m) reference paper sizes applicable to the Chinese National Standard (CNS) A4 specification (210 x 297 degrees) 之方法,其中,在 之比值(Rk)值係已 額外之取出點所產 偶合與非線性爭溫線之知識模式,Μ y. . . .μ . ^ 飞例如二_極限之選擇 性值或通式化(藍穆爾_富羅英 夹仏利奇等溫線係使用於 分離系統弋模擬。 1 1 ·根據申請專利範園第1至3項中杯 、 T仕—項弋方法,其中在包 括某數目Ρ之區域數之分離迴路申 丄、 略Τ &lt;比值(Rk)值係已知 的,由在分離迴路中飼人至少—個額外之注人點所產主 之額外比值之對應值’係決定成在鄰近區域中之比值值 與在該額外注入點之注入流量值之函 I2·根據申請專利範園第1至3項中任一項 包括某數目p之區域數之分離迴路中 知的,由在分離迴路中飼入至少一個 / ll~f ✓ I ^ 生之額外比值之對應值,係決定成在鄰近區域中之比值 值與在該額外取出點之取出流量值之函數。 13. 根據申請專利範圍第8項之方法,其中係選擇取出流體 中之組份濃度間之比值以作為被控制變數。 14. 根據申請專利範圍第項中任一項之方法其中係選 擇一最適化演算法0^·被控制變數允許經由固定之次 序以達到。 15·根據前述申請專利一項之方法,其係應用於具 女 ' Λη —I» — … “ 二〆、 -3 本紙張尺度適用中國國家標準(CNS ) Α4現格(210X297公釐) IT.— m n^— 1 m (n mu I. 1 n n nn--eJ (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 有八個碳原子的芳香分離 經濟部中央標準局員工消費合作社印製 A8 Βδ C8 D8 六、申請專利把圍 數。 5 .根據申請專利範園第2項之方法,其中,在含有包括η區 且鄰接之階段之陣列之該分離迴路區域上,其中定義出 η個比值(Rk) ’包含根據流量值(D)與濃度值(X)定義出m 個被控制變數(ξ )’其m值係小於或等於η值,測量在區 段之端點處於液相中之濃度且決定m該比值(Rk)或該比 值之m合併,其含有(n-m)個參數。 6 .根據申清專利範圍第1至3項中任一項之方法,其中該操 作變數係流量且閥變換期(T)係可模擬塔床之排代。 7 .根據申請專利範圍第1至3項中任一項之方法,其中該分 離迴路係包括四個主要之區域、且從各個濃度之線上測 量同時控制例如為迴路之產率以及混合物之至少一個組 份之純度之被控制變數(ξ)。 8 .根據申請專利範圍第1至3項中任一項之方法,、其中係含 有藉扛曼(Raman)式之線上分析、色層分析或近紅外線 (NIR)分析進行之濃度測量。 9 .根據申請專利範圍第1至3項中任一項之方法,其中,在 具有四個區域之分離系統之例子中,係選擇下述四個量 中之至少一個以作為被控制變數:從迴路所取出之流體 中之第一組份之純度、分離系統對一組份之產率、該第 —組份在與流體之循環方向有關之此四區之第一者之後 部之尾量、或除了該第一組份外所有組份之尾量,其係 在與流體之循環方向有關之此四區之最後者之前部。 10.根據申請專利範圍第1至3項中任—項之方法,其係基於 ( CNS ) A4^ ( 210X297,JiT*~-^- (請先閲讀背面之注項再填寫本頁) 衣. 訂The method, in which the ratio (Rk) value is the knowledge model of the coupling and non-linear temperature line produced by the additional extraction point, M y.... Μ. Generalization (Lam Moore_Fuluoying Jialiqi Isotherm is used in the separation system 弋 simulation. 1 1 · According to the patent application Fanyuan No. 1 to 3 medium cup, T Shi-Xiang 弋 method, where In the separation circuit that includes a certain number of P regions, the value of the &lt; Tk &lt; ratio (Rk) is known and the ratio of the extra ratio of the owner produced by feeding at least one additional injection point in the separation circuit. Corresponding value 'is determined as a function of the ratio between the adjacent area and the injection flow value at the additional injection point. I2. According to any of the items 1 to 3 of the patent application park, the number of areas including a certain number of p is separated. Known in the circuit, the corresponding value of the additional ratio of feed at least one / ll ~ f ✓ I ^ in the separation circuit is determined as the ratio of the ratio in the adjacent area to the value of the extraction flow at the additional extraction point Function 13. Method according to item 8 of the patent application, where Select the ratio between the component concentrations in the fluid to be taken out as the controlled variable. 14. According to the method of any one of the scope of the patent application, an optimization algorithm is selected. 0 ^ The controlled variables are allowed to pass through a fixed order. 15. The method according to one of the aforementioned patent applications, which is applied to Gu Nu 'Λη —I »—…“ Erji, -3 This paper is applicable to the Chinese National Standard (CNS) A4 (210X297 mm) ) IT.— mn ^ — 1 m (n mu I. 1 nn nn--eJ (Please read the notes on the back before filling out this page) Employees' Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs printed an aroma with eight carbon atoms Printed by A8, Bδ, C8, D8, Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs 6. Number of patent applications. 5. The method according to item 2 of the patent application park, in which the On the separation loop area, η ratios (Rk) are defined, including m controlled variables (ξ) are defined according to the flow value (D) and concentration value (X), whose m value is less than or equal to the η value, measuring The concentration at the end of the segment is in the liquid phase and determines the ratio m (Rk) or the combination of the ratio m, which contains (nm) parameters. 6. According to any of the claims 1 to 3 in the scope of the patent application Method, wherein the operating variable is the flow rate and the valve transition period (T) can simulate the replacement of the tower bed. 7. The method according to any one of the claims 1 to 3, wherein the separation circuit includes Four main areas, and measured from the line of each concentration, simultaneously control, for example, the yield of the loop and the controlled variable (ξ) of the purity of at least one component of the mixture. 8. The method according to any one of claims 1 to 3, which includes concentration measurement by Raman-type online analysis, chromatographic analysis, or near-infrared (NIR) analysis. 9. The method according to any one of the claims 1 to 3, wherein, in the example of a separation system having four regions, at least one of the following four quantities is selected as the controlled variable: from The purity of the first component in the fluid taken out by the circuit, the yield of the component by the separation system, the tail of the first component behind the first of the four zones related to the circulation direction of the fluid, Or the tails of all the components except the first component are in front of the last of the four zones related to the circulation direction of the fluid. 10.According to the method of any one of items 1 to 3 of the scope of patent application, it is based on (CNS) A4 ^ (210X297, JiT * ~-^-(Please read the note on the back before filling this page). Order 之方法,其中,在 之比值(Rk)值係已 額外之取出點所產 偶合與非線性爭溫線之知識模式,Μ y. . . .μ . ^ 飞例如二_極限之選擇 性值或通式化(藍穆爾_富羅英 夹仏利奇等溫線係使用於 分離系統弋模擬。 1 1 ·根據申請專利範園第1至3項中杯 、 T仕—項弋方法,其中在包 括某數目Ρ之區域數之分離迴路申 丄、 略Τ &lt;比值(Rk)值係已知 的,由在分離迴路中飼人至少—個額外之注人點所產主 之額外比值之對應值’係決定成在鄰近區域中之比值值 與在該額外注入點之注入流量值之函 I2·根據申請專利範園第1至3項中任一項 包括某數目p之區域數之分離迴路中 知的,由在分離迴路中飼入至少一個 / ll~f ✓ I ^ 生之額外比值之對應值,係決定成在鄰近區域中之比值 值與在該額外取出點之取出流量值之函數。 13. 根據申請專利範圍第8項之方法,其中係選擇取出流體 中之組份濃度間之比值以作為被控制變數。 14. 根據申請專利範圍第項中任一項之方法其中係選 擇一最適化演算法0^·被控制變數允許經由固定之次 序以達到。 15·根據前述申請專利一項之方法,其係應用於具 女 ' Λη —I» — … “ 二〆、 -3 本紙張尺度適用中國國家標準(CNS ) Α4現格(210X297公釐) IT.— m n^— 1 m (n mu I. 1 n n nn--eJ (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 有八個碳原子的芳香分離The method, in which the ratio (Rk) value is the knowledge model of the coupling and non-linear temperature line produced by the additional extraction point, M y.... Μ. Generalization (Lam Moore_Fuluoying Jialiqi Isotherm is used in the separation system 弋 simulation. 1 1 · According to the patent application Fanyuan No. 1 to 3 medium cup, T Shi-Xiang 弋 method, where In the separation circuit that includes a certain number of P regions, the value of the &lt; Tk &lt; ratio (Rk) is known and the ratio of the extra ratio of the owner produced by feeding at least one additional injection point in the separation circuit. Corresponding value 'is determined as a function of the ratio between the adjacent area and the injection flow value at the additional injection point. I2. According to any of the items 1 to 3 of the patent application park, the number of areas including a certain number of p is separated. Known in the circuit, the corresponding value of the additional ratio of feed at least one / ll ~ f ✓ I ^ in the separation circuit is determined as the ratio of the ratio in the adjacent area to the value of the extraction flow at the additional extraction point Function 13. Method according to item 8 of the patent application, where Select the ratio between the component concentrations in the fluid to be taken out as the controlled variable. 14. According to the method of any one of the scope of the patent application, an optimization algorithm is selected. 0 ^ The controlled variables are allowed to pass through a fixed order. 15. The method according to one of the aforementioned patent applications, which is applied to Gu Nu 'Λη —I »—…“ Erji, -3 This paper is applicable to the Chinese National Standard (CNS) A4 (210X297 mm) ) IT.— mn ^ — 1 m (n mu I. 1 nn nn--eJ (Please read the notes on the back before filling out this page) Employees' Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs printed an aroma with eight carbon atoms Separate
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CN111629802A (en) * 2017-11-16 2020-09-04 诺瓦塞普工艺公司 Method for conditioning a separation mixture

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111629802A (en) * 2017-11-16 2020-09-04 诺瓦塞普工艺公司 Method for conditioning a separation mixture
US11857892B2 (en) 2017-11-16 2024-01-02 Novasep Process Solutions Regulated method for separating a mixture

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