JP2962589B2 - Simulated moving bed chromatographic separator - Google Patents
Simulated moving bed chromatographic separatorInfo
- Publication number
- JP2962589B2 JP2962589B2 JP3101643A JP10164391A JP2962589B2 JP 2962589 B2 JP2962589 B2 JP 2962589B2 JP 3101643 A JP3101643 A JP 3101643A JP 10164391 A JP10164391 A JP 10164391A JP 2962589 B2 JP2962589 B2 JP 2962589B2
- Authority
- JP
- Japan
- Prior art keywords
- liquid
- valve
- raffinate
- extracting
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、２成分以上の成分を含
む原液中の特定成分に対して選択的吸着能力を有する吸
着剤を充填した多数の単位充填塔を、直列かつ無端に連
結して、擬似移動層式クロマト分離を行なうようにした
装置に関するものである。BACKGROUND OF THE INVENTION The present invention relates to a series of endlessly connected unit packed columns packed with an adsorbent having a selective adsorption capacity for a specific component in a stock solution containing two or more components. And an apparatus for performing simulated moving bed type chromatographic separation.
【０００２】[0002]
【従来の技術】擬似移動層式クロマト分離装置は、代表
的には原液中に含まれる２成分以上の成分中の特定成分
に対して選択的吸着能力を有する吸着剤を充填した多数
の単位充填塔（以下単に充填塔という）を配管で直列に
連結すると共に、最後部の充填塔と最前部の充填塔を配
管で連結することによって、全体を無端に連結した充填
塔群の系として形成させた装置において、原液の供給、
溶離液の供給、及びラフィネート液の抜き出し、エクス
トラクト液の抜き出しの各位置関係を一定に保ちながら
これらの位置を経時的に下流側に移行させることで、吸
着剤の実際の移動を行なわずに移動層の処理操作を擬似
的に実現する装置であることはよく知られている。この
ような代表的装置においては、液が流れている系内の充
填塔群が、その液流れの方向に沿って上流側から下流側
に向かって各成分が富豊化された第１区画、第２区画、
第３区画、第４区画に分かれる（すなわち吸着剤に対し
て各成分の富豊化された領域が分れる）ので、その第１
区画の最前列の充填塔の入口から溶離液を供給すると共
に、第３区画の最前列に位置する充填塔の入口から原液
を供給し、さらに第３区画の最後列に位置する充填塔の
出口から被吸着成分の少ないラフィネート液を抜き出す
と共に、第１区画の最後列に位置する充填塔の出口から
被吸着成分の含有量の多いエクストラクト液を抜き出
し、上記富豊化された各成分の領域の進行に伴ってこれ
らの液供給位置と液抜き出し位置を下流側に移行させる
ように操作して各成分を回収する。2. Description of the Related Art A simulated moving bed type chromatographic separation apparatus typically includes a large number of unit packings filled with an adsorbent having a selective adsorption ability for a specific component of two or more components contained in a stock solution. By connecting the towers (hereinafter simply referred to as packed towers) in series with pipes and connecting the last packed tower and the frontmost packed tower with pipes, the whole is formed as a system of packed towers connected endlessly. Supply of undiluted solution,
The positions of the eluent supply, the extraction of the raffinate solution, and the extraction solution are kept constant, and these positions are shifted to the downstream side over time so that the adsorbent does not actually move. It is well known that the device is a device that simulates a moving layer processing operation. In such a typical apparatus, the packed tower group in the system in which the liquid flows is a first section in which each component is enriched from the upstream side to the downstream side along the direction of the liquid flow, The second section,
It is divided into a third section and a fourth section (that is, a region where each component is enriched with respect to the adsorbent is separated).
The eluent is supplied from the inlet of the packed tower in the front row of the section, the undiluted solution is supplied from the inlet of the packed tower located in the front row of the third section, and the outlet of the packed tower located in the last row of the third section. , A raffinate liquid having a small amount of the component to be adsorbed is extracted from the column, and an extract liquid having a large content of the component to be adsorbed is extracted from the outlet of the packed tower located in the last row of the first section. Each component is recovered by operating the liquid supply position and the liquid extraction position to shift to the downstream side as the process proceeds.
【０００３】そして、このような充填塔群の系に対する
液の供給と抜き出しという物質収支を不都合なく維持す
るために、積極的な液フィードが必要な供給側だけでな
く、ラフィネート液やエクストラクト液を抜き出す側に
も、流量が自動制御できるポンプや自動制御可能な流量
コントロール弁を設け、系内の圧力が上がりすぎたり下
がりすぎたりしない様にして一定流量で正確な液抜き出
しを行なっている。[0003] In order to maintain the material balance of supply and withdrawal of the liquid to such a packed tower group system without any inconvenience, not only the supply side which needs a positive liquid feed but also the raffinate liquid and the extract liquid. A pump capable of automatically controlling the flow rate and a flow control valve capable of automatically controlling are also provided on the side from which the liquid is extracted, so that the liquid in the system is accurately discharged at a constant flow rate so that the pressure in the system does not rise or fall too much.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、前述し
た擬似移動層式クロマト分離装置における液抜き出しの
ために用いられる流量制御可能なポンプ、あるいは自動
制御可能な流量コントロール弁は、抜き出し量を正確に
保つために高性能で高価なものが必要であるという難点
があった。また、液抜き出しにピストン往復動型ポンプ
を２台用いることもできるが、系内圧力を一定に保つた
めに一方のポンプは頻繁にモーターの回転数を例えば各
カラムの頂部に設けた圧力検知装置の検出値の平均値に
基づいて可変制御することが必要なため、ポンプの消耗
が早く、耐久性に問題があった。そしてこの傾向は、上
記ポンプに代用できるような適切な大きさの自動制御可
能な流量コントロール弁が一般に供給されていない小流
量用が必要となる小型装置の場合に、特に顕著な問題と
なっている。However, the flow controllable pump or the automatically controllable flow control valve used for liquid extraction in the simulated moving bed type chromatographic separation apparatus described above keeps the extraction amount accurate. Therefore, there is a problem that a high-performance and expensive one is required. In addition, two piston reciprocating pumps can be used for liquid extraction, but in order to keep the pressure in the system constant, one of the pumps frequently changes the number of rotations of the motor, for example, a pressure detection device provided at the top of each column. Since it is necessary to perform variable control based on the average value of the detected values, the pump is quickly consumed and there is a problem in durability. This tendency becomes a particularly significant problem in the case of a small device that requires a small flow rate, in which an automatically controllable flow control valve of an appropriate size that can be substituted for the pump is not generally supplied. I have.
【０００５】以上のような観点から、本発明者は種々研
究を重ね、制御が簡単で安価な擬似移動層式クロマト分
離装置を提供することを目的として本発明を開発するに
至ったものである。In view of the above, the present inventors have conducted various studies and have developed the present invention for the purpose of providing an inexpensive simulated moving bed type chromatographic separation apparatus which is easy to control. .
【０００６】本発明の他の目的は、長期間安定な運転の
できる擬似移動層式クロマト分離装置を提供することに
ある。特に、ピストン往復動型ポンプの使用が避けられ
ない小型の装置において、安定な運転が長期間に渡って
実現できる擬似移動層式クロマト分離装置を提供するこ
とにある。Another object of the present invention is to provide a simulated moving bed type chromatographic separation apparatus which can be operated stably for a long period of time. In particular, it is an object of the present invention to provide a simulated moving bed type chromatographic separation apparatus capable of realizing stable operation for a long period of time in a small apparatus in which use of a piston reciprocating pump cannot be avoided.
【０００７】[0007]
【課題を解決するための手段及び作用】本発明者は、以
上のような目的を達成するために、吸着剤が充填されて
いる複数の充填塔を無端直列に連結した系と、これらの
充填塔のいずれかを選択して原液を供給する原液供給手
段と、他のいずれかの充填塔を選択して溶離液を供給す
る溶離液供給手段と、いずれかの充填塔を選択してラフ
ィネート液を上記系外に抜き出す第１の液抜き出し手段
と、他のいずれかの充填塔を選択してエクストラクト液
を系外に抜き出す第２の液抜き出し手段と、系内におけ
る上記液の供給及び抜き出しの位置関係を相互に維持し
て、これらの位置を系内の液流れ方向の下流側に順次移
行させる切換制御手段と、を備えた擬似移動層式クロマ
ト分離装置において、上記第１の液抜き出し手段又は第
２の液抜き出し手段のいずれか一方には抜き出し液の流
量をコントロールする流量制御手段を設けると共に、こ
れらの第１の液抜き出し手段又は第２の液抜き出し手段
のいずれか他方には、抜き出し上流側に予め定めた一定
圧の背圧を与える背圧付与手段を設けたことを特徴とす
る本発明の擬似移動層式クロマト分離装置を完成した。In order to achieve the above objects, the present inventor has set forth a system in which a plurality of packed towers filled with an adsorbent are connected endlessly in series, A stock solution supply means for selecting one of the columns and supplying a stock solution, an eluent supply means for selecting one of the other packed towers and supplying an eluent, and a raffinate solution by selecting one of the packed towers Liquid extracting means for extracting the extracted liquid out of the system, second liquid extracting means for selecting any other packed tower to extract the extract liquid out of the system, supply and extraction of the liquid in the system And a switching control means for sequentially shifting these positions to the downstream side in the liquid flow direction in the system while maintaining the mutual positional relationship between the first and second liquids. Means or second drainer Is provided with a flow rate control means for controlling the flow rate of the withdrawal liquid, and the other of the first liquid withdrawal means and the second liquid withdrawal means is provided with a predetermined flow rate upstream of the withdrawal liquid. A simulated moving bed type chromatographic separation apparatus according to the present invention, wherein a back pressure applying means for applying a back pressure of pressure is provided.
【０００８】本発明は、原液中に含まれる２成分以上の
成分中の特定成分に対して選択的吸着能力を有する吸着
剤を充填した多数の充填塔を配管で直列に連結すると共
に、最後部の充填塔と最前部の充填塔をも配管で連結す
ることによって無端に連結した充填塔群を形成し、該充
填塔群を上流側から下流側に向かって第１区画、第２区
画、第３区画、第４区画に区画し、第１区画の最前列に
位置する充填塔の入口から溶離液を供給弁を介して供給
すると共に、第３区画の最前列に位置する充填塔の入口
から原液を供給弁を介して供給し、かつ第３区画の最後
列に位置する充填塔の出口から被吸着成分の少ないラフ
ィネート液を抜き出し弁を介して抜き出すと共に、第１
区画の最後列に位置する充填塔の出口から被吸着成分の
含有量の多いエクストラクト液を抜き出し弁を介して抜
き出し、これらの溶離液の供給位置、原液の供給位置、
ラフィネート液の抜き出し位置、エクストラクト液の抜
き出し位置を、上記原液中の成分の吸着剤に対する吸着
領域の移行に伴って下流側に繰り下げるように操作され
る擬似移動層式クロマト分離装置に対して最も代表的に
適用されるが、特にこれに限定されるものではなく、例
えば、本出願人が特願昭６０−２２８８０６号（特開昭
６２−９１２０５号）により提案した擬似移動層式装置
等、本発明の要旨を損なわないものであれば他の形式の
擬似移動層式クロマト分離装置にも適用できる。According to the present invention, a plurality of packed towers filled with an adsorbent having a selective adsorption ability for a specific component of two or more components contained in a stock solution are connected in series by piping, and The packed tower and the foremost packed tower are also connected by pipes to form a packed tower group connected endlessly, and the packed tower group is divided from the upstream side to the downstream side in the first section, the second section, and the second section. The eluent is supplied through a supply valve from the inlet of the packed tower located in the front row of the first section, and the eluent is supplied from the inlet of the packed tower located in the front row of the third section. The undiluted solution is supplied through a supply valve, and a raffinate solution having a small amount of components to be adsorbed is extracted from an outlet of a packed tower located in the last row of the third section through an extraction valve.
Extract liquid having a high content of the component to be adsorbed is extracted from the outlet of the packed tower located in the last row of the section through an extraction valve, and the supply position of these eluents, the supply position of the undiluted solution,
With respect to the simulated moving bed type chromatographic separation apparatus, the extraction position of the raffinate liquid and the extraction position of the extract liquid are moved down to the downstream side in accordance with the shift of the adsorption region of the components in the stock solution to the adsorbent. Although it is typically applied, the present invention is not particularly limited thereto. For example, a simulated moving bed type device proposed by the present applicant in Japanese Patent Application No. 60-228806 (Japanese Patent Application Laid-Open No. 62-91205), and the like. As long as the gist of the present invention is not impaired, the present invention can be applied to another type of simulated moving bed type chromatographic separation apparatus.
【０００９】本発明を適用して構成される擬似移動層式
クロマト分離装置は、一般に配管の配設をできるだけ省
略，短尺化することが求められる実装置においては、ラ
フィネート抜き出し弁を介設したラフィネート液抜き出
し用配管を用いて、それぞれの充填塔と共通のラフィネ
ート液抜き出し用合流管を接続連結し、同様に、エクス
トラクト抜き出し弁を介設したエクストラクト液抜き出
し用配管を用いて、それぞれの充填塔と共通のエクスト
ラクト液抜き出し用合流管を接続連結した装置におい
て、これらの合流管に、上記流量制御手段及び背圧付与
手段を設ける形式のものとして構成される。In a simulated moving bed type chromatographic separation apparatus constructed by applying the present invention, in general, it is required to reduce the piping arrangement as much as possible and to shorten the length thereof. Each of the packed towers is connected and connected to a common raffinate liquid extraction merging pipe using liquid extraction pipes, and similarly, each filling tower is connected to an extraction liquid extraction pipe provided with an extraction extraction valve. In an apparatus in which a column and a common extract liquid extraction merging pipe are connected and connected, these merging pipes are provided with the flow rate control means and the back pressure applying means.
【００１０】本発明において使用される背圧付与手段
は、目的とする一定圧の背圧を液抜き出し管の上流側に
与えることができるものであれば、構造を特に限定され
るものではないが、一般的には、背圧弁、逃がし弁、安
全弁、ニードル弁、オリフィス、抵抗管等のものを用い
ることができ、このような背圧付与手段によって付与す
る背圧の大きさは、装置の構造や規模等によっても異な
るが、一般的には１〜５ｋｇ／ｃｍ2 Ｇ程度とされる。The structure of the back pressure applying means used in the present invention is not particularly limited as long as it can apply a desired constant back pressure to the upstream side of the liquid discharge pipe. Generally, a back pressure valve, a relief valve, a safety valve, a needle valve, an orifice, a resistance pipe, or the like can be used. The magnitude of the back pressure applied by such back pressure applying means depends on the structure of the device. In general, it is about 1 to 5 kg / cm @ 2 G, though it varies depending on the size and the scale.
【００１１】本発明は、ラフィネート液の抜き出し配管
又はエクストラクト液の抜き出し配管のいずれか一方に
設ける流量制御手段として、適当な流量コントロール弁
が一般的に存在しないために流量制御可能のポンプを用
いなければならない形式の比較的小型の擬似移動層式ク
ロマト分離装置において特に好適で、優れた効果を発揮
し、一般的には液抜き出し用の配管が２５ｍｍ径以下、
より現実的には１０ｍｍ径以下、特には４〜５ｍｍ径以
下の場合に、従来構成では困難であった本発明の効果を
奏する装置を提供できる。このような小型の装置が適用
される具体的な用途としては、種々の生化学分野におい
て得られる生体からの分離液，培養液等から酵素や蛋白
質等の生理活性物質を分離回収する用途、比較的少量の
溶液から化学物質を分離する医薬，ファインケミカル等
の分野、酵素反応液等から有用物質を分離回収する分野
等々を例示することができる。According to the present invention, a pump capable of controlling the flow rate is used as a flow rate control means provided in one of the pipe for extracting the raffinate liquid and the pipe for extracting the extract liquid, since there is generally no suitable flow control valve. It is particularly suitable for relatively small simulated moving bed type chromatographic separators of the type that must be used, and exhibits excellent effects. Generally, the pipe for liquid extraction is 25 mm or less in diameter,
More practically, when the diameter is 10 mm or less, particularly 4 to 5 mm or less, it is possible to provide a device that can achieve the effects of the present invention, which has been difficult with the conventional configuration. Specific applications to which such a small device is applied include the use for separating and recovering physiologically active substances such as enzymes and proteins from separated liquids and cultures from living organisms obtained in various biochemical fields, Examples include fields such as pharmaceuticals and fine chemicals for separating chemical substances from a very small amount of solution, and fields for separating and recovering useful substances from enzyme reaction solutions and the like.
【００１２】[0012]
【発明の効果】本発明の装置によれば、擬似移動層式ク
ロマト分離装置における二つの液抜き出し配管のいずれ
か一方に流量制御が可能なポンプ等を設け、これらのい
ずれか他方に背圧弁、逃がし弁、安全弁などを設けてそ
の作動圧を設定するか、ニードル弁を設けてその開度を
設定するか、適切なオリフィスまたは抵抗管を取り付け
ることで一定圧の背圧を付与するだけで、原液供給量と
溶離液供給量の和からポンプまたはコントロール弁によ
って抜き出されるエクストラクト液（またはラフィネー
ト液）の量を差引いた分を、ラフィネート液（またはエ
クストラクト液）として、該流出弁の入口側の圧力を高
すぎることなくかつ低すぎることなく抜き出すことが可
能となり、従来のこの種の装置において必要とされてい
た自動制御可能な流量可変型のポンプあるいは自動制御
可能なコントロール弁を、１台減らすことができると共
に、これに付属する流量制御が可能なポンプ等の流量を
自動制御をするための検出機構、自動制御機構そのもの
を不要とすることができる効果がある。According to the apparatus of the present invention, a pump or the like capable of controlling the flow rate is provided in one of the two liquid extraction pipes in the simulated moving bed type chromatographic separator, and the back pressure valve and By providing a relief valve, a safety valve, etc. to set its operating pressure, by providing a needle valve and setting its opening, or by attaching a suitable orifice or resistance tube, simply applying a constant pressure back pressure, The amount obtained by subtracting the amount of the extract liquid (or the raffinate liquid) extracted by the pump or the control valve from the sum of the supply amount of the undiluted liquid and the supply amount of the eluent is defined as the raffinate liquid (or the extract liquid), Side pressure can be withdrawn without being too high and without being too low. The number of variable-volume pumps or automatically controllable control valves can be reduced by one, and the detection mechanism and the automatic control mechanism itself for automatically controlling the flow rate of the pumps that can control the flow rate attached to this pump can be reduced. There is an effect that can be made unnecessary.
【００１３】また本発明の装置は、長期間安定な運転が
できるという効果もある。The device of the present invention also has an effect that stable operation can be performed for a long time.
【００１４】更に又本発明の装置は、自動制御可能なコ
ントロール弁が使用できないような小型の装置に特に好
適で、この種の装置では従来にない安定な運転が長期間
に渡って実現できる効果がある。Further, the device of the present invention is particularly suitable for a small device in which a control valve which can be automatically controlled cannot be used. This type of device can achieve an unprecedented stable operation for a long period of time. There is.
【００１５】[0015]
【実施例】以下本発明を実施例に基づいて詳細に説明す
るが、本発明がこれらの実施例に限定されるものでない
ことは当然である。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described in detail below with reference to embodiments, but it is needless to say that the present invention is not limited to these embodiments.
【００１６】実施例１（マルトースとマルトトリオース
の分離） 第１図は本実施例に使用した装置のフローを示す説明図
である。Embodiment 1 (Separation of Maltose and Maltotriose) FIG. 1 is an explanatory diagram showing the flow of the apparatus used in this embodiment.
【００１７】内径３．７ｃｍ、長さ５０ｃｍの充填塔Ｃ
（Ｃ１．．．．Ｃ８）８本のそれぞれの末端を、次の充
填塔の頂部に配管Ｈで無端連結し、配管Ｈの上流側にラ
フィネート液抜き出し弁Ａ（Ａ１，・・・・，Ａ８）及
びエクストラクト液抜き出し弁Ｂ（Ｂ１，・・・・，Ｂ
８）を連結すると共に、配管Ｈの下流側にポンプＰ３に
よって供給される原液フィード管Ｆから分岐した原液供
給弁Ｆ（Ｆ１，・・・・，Ｆ８）と、ポンプＰ２によっ
て供給される溶離液フィード管Ｄから分岐した溶離液供
給弁Ｄ（Ｄ１，・・・・，Ｄ８）を連結し、充填塔Ｃ８
の末端から充填塔Ｃ１の頂部への配管の途中に循環ポン
プＰ１を連結し、さらに各エクストラクト液抜き出し弁
Ｂ１〜Ｂ８を合流管Ｅに接続してこの下流出口側にエク
ストラクト液抜き出しポンプＰ４を連結し、各ラフィネ
ート液抜き出し弁Ａ１〜Ａ８を合流管Ｒに接続してこの
下流出口側に直列に背圧弁Ａ９を取り付けた装置を構成
した。なお背圧弁の作動圧は０．３ＭＰａとした。Packing tower C having an inner diameter of 3.7 cm and a length of 50 cm
(C1 ... C8) The ends of each of the eight pipes are endlessly connected to the top of the next packed tower by a pipe H, and a raffinate liquid extraction valve A (A1,..., A8) is provided upstream of the pipe H. ) And extract liquid extraction valve B (B1,..., B
8), a stock solution supply valve F (F1,..., F8) branched from a stock solution feed pipe F supplied by a pump P3 to the downstream side of the pipe H, and an eluent supplied by a pump P2. An eluent supply valve D (D1,..., D8) branched from a feed pipe D is connected to a packed tower C8.
A circulation pump P1 is connected to the middle of the pipe from the end of the packing tower C1 to the top of the packed tower C1, and each of the extract liquid extracting valves B1 to B8 is connected to the junction pipe E, and the extract liquid extracting pump P4 is connected to the downstream outlet side. And the raffinate liquid extraction valves A1 to A8 were connected to a merging pipe R, and a back pressure valve A9 was attached in series at the downstream outlet side. The operating pressure of the back pressure valve was 0.3 MPa.
【００１８】また上記各充填塔には強酸性カチオン交換
樹脂アンバーライトＣＧ−６０００のＮａ型を充填し、
ポンプには分取クロマト用のピストン往復動型を用い
た。Each of the packed columns is packed with a strong acid cation exchange resin Amberlite CG-6000 Na type,
The pump used was a piston reciprocating type for preparative chromatography.
【００１９】以上の構成の装置において、第１の工程と
して、原液供給弁Ｆ５を開いて充填塔Ｃ５の頂部から原
液として粗製マルトース液を導入し、溶離液供給弁Ｄ１
を開いて充填塔Ｃ１の頂部から溶離液として水を導入
し、またラフィネート液抜き出し弁Ａ６を開いて充填塔
Ｃ６の底部からマルトトリオースを多く含む液（ラフィ
ネート液）を抜き出し、エクストラクト液抜き出し弁Ｂ
２を開いて充填塔Ｃ２の底部からマルトースを多く含む
液（エクストラクト液）を抜き出し、更に充填塔Ｃ８の
底部からの液を循環ポンプＰ１を介して充填塔Ｃ１の頂
部に導入した。In the apparatus having the above-described structure, as a first step, the raw liquid supply valve F5 is opened to introduce a crude maltose liquid as a raw liquid from the top of the packed tower C5, and the eluent liquid supply valve D1
Is opened to introduce water as an eluent from the top of the packed tower C1, and a raffinate liquid extraction valve A6 is opened to extract a liquid containing a large amount of maltotriose (raffinate liquid) from the bottom of the packed tower C6, and to extract an extract liquid. Valve B
2, the liquid containing much maltose (extract liquid) was extracted from the bottom of the packed tower C2, and the liquid from the bottom of the packed tower C8 was introduced into the top of the packed tower C1 via the circulation pump P1.
【００２０】予め定めた時間を経過した後、第２工程と
して、上記第１工程で開とした原液供給弁Ｆ５を閉じか
つ原液供給弁Ｆ６を開き、同様にして溶離液供給弁の開
をＤ１からＤ２へ切換え、ラフィネート液抜き出し弁の
開をＡ６からＡ７へ切換え、エクストラクト液抜き出し
弁の開をＢ２からＢ３へ切換えた。After a lapse of a predetermined time, as a second step, the stock solution supply valve F5 opened in the first step is closed and the stock solution supply valve F6 is opened. To D2, the opening of the raffinate liquid extraction valve was switched from A6 to A7, and the extraction liquid extraction valve was switched from B2 to B3.
【００２１】以下同様にして、上記の一定時間毎に、開
とする弁を順次液の流れ方向の下流側に移行させる操作
を行なった。In the same manner as described above, the operation of sequentially moving the valve to be opened to the downstream side in the liquid flow direction was performed at regular intervals as described above.
【００２２】原液組成、運転条件を下に記す。The composition of the stock solution and the operating conditions are described below.
【００２３】 原液 固形分濃度 ４９．４％ 組成 マルトテトラオース ５．８％ マルトトリオース １２．５％ マルトース ７７．２％ グルコース ４．５％ 移動周期 ６．２５ｍｉｎ／工程 溶離液供給量 ８．４８ｍｌ／ｍｉｎ 原液供給量 ２．１２ｍｌ／ｍｉｎ エクストラクト液流出量 ４．９５ｍｌ／ｍｉｎ ラフィネート液流出量 ５．６５ｍｌ／ｍｉｎ （ただし、背圧弁を通して抜き出されるラフィネート液
の流出量は、原液及び溶離液の供給量からエクストラク
ト液流出量を減算した計算値であり、ピストン往復動型
のポンプを通して抜き出されるエクストラクト液の流出
量は、 該ポンプを一定値に設定して流量の可変制御は
行なわなかった。） 循環ポンプ流量（設定値） 第１、２工程 ３１．６ ｍｌ／ｍｉｎ 第３、４工程 ３７．３ ｍｌ／ｍｉｎ 第５、６工程 ３５．１ ｍｌ／ｍｉｎ 第７、８工程 ４０．１ ｍｌ／ｍｉｎ 弁の開閉を第１の充填塔から第８の充填塔まで切換える
操作を１サイクルとして連続して行なったところ、数十
サイクルに渡って安定した操作を行なうことができ、数
十サイクル後に抜き出されたラフィネート液及びエクス
トラクト液の組成も下記表１に示したように安定してい
た。Undiluted solution Solid concentration 49.4% Composition Maltotetraose 5.8% Maltotriose 12.5% Maltose 77.2% Glucose 4.5% Transfer cycle 6.25 min / step Eluent supply 8.48 ml / Min Stock solution supply 2.12 ml / min Extract solution outflow 4.95 ml / min Raffinate solution outflow 5.65 ml / min (However, the outflow of the raffinate solution extracted through the back pressure valve depends on the stock solution and the eluate. This is a calculated value obtained by subtracting the extract liquid outflow amount from the supply amount, and the extract liquid outflow amount extracted through the piston reciprocating pump is set to a constant value and the flow rate is not variably controlled. The circulation pump flow rate (set value) 31.6 ml / min for the first and second steps 31.6 ml / min for the third and fourth steps 1 / min 5th and 6th steps 35.1 ml / min 7th and 8th steps 40.1 ml / min The operation of switching the opening and closing of the valve from the first packed tower to the eighth packed tower is continuously performed as one cycle. As a result, stable operations could be performed over several tens of cycles, and the compositions of the raffinate solution and the extract solution extracted after several tens of cycles were also stable as shown in Table 1 below.
【００２４】[0024]
【表１】 [Table 1]
【００２５】比較例（マルトースとマルトトリオースの
分離） 第３図は本比較例に使用した装置のフローを示す説明図
である。Comparative Example (Separation of Maltose and Maltotriose) FIG. 3 is an explanatory diagram showing the flow of the apparatus used in this comparative example.
【００２６】本例においては、ラフィネート液抜き出し
弁の出口側に系内圧を一定に保つように、各カラムの頂
部に設けた圧力検知装置の検出値の平均値に基づいて可
変制御されるラフィネート液抜き出しポンプＰ５を取り
付けた点が異なる他は、実施例１と同様の構成の装置を
用い、実施例の装置と同様の操作を行なった。In this embodiment, the raffinate liquid is variably controlled based on the average of the detection values of the pressure detecting devices provided at the top of each column so as to keep the system pressure constant at the outlet side of the raffinate liquid extraction valve. An apparatus having the same configuration as in Example 1 was used, except that the extraction pump P5 was attached, and the same operation as the apparatus in Example was performed.
【００２７】原液組成、運転条件を下記に示す。なおエ
クストラクト液の流出量は、エクストラクト液抜き出し
ポンプＰ４の流量を一定値に設定して流量の可変制御は
行なわず、ラフィネート液抜き出しポンプＰ５は、上述
の如く各充填塔に設けた圧力検知装置の検出値の平均値
に基づいて可変制御した。The composition of the stock solution and the operating conditions are shown below. The flow rate of the extract liquid was determined by setting the flow rate of the extract liquid extraction pump P4 to a constant value, and the flow rate was not variably controlled. The raffinate liquid extraction pump P5 was controlled by the pressure detection provided in each packed tower as described above. Variable control was performed based on the average of the detected values of the device.
【００２８】 数十サイクル後の流出液の組成は下記表２の通りであ
ったが、３７サイクルでラフィネート抜き出しポンプＰ
５が故障した。これは流量制御による消耗のためと判断
された。[0028] The composition of the effluent after several tens of cycles was as shown in Table 2 below.
5 failed. This was determined to be due to exhaustion due to flow control.
【００２９】[0029]
【表２】 [Table 2]
【００３０】実施例２ 第２図に示した本例は、第１図に示した充填塔群Ｃの系
内に循環ポンプを設けることに代えて、該系の配管から
分岐した独立の循環ライン配管Ｊとその途中の循環ポン
プＰ１１とを設け、例えば充填塔Ｃ１から順次Ｃ２・・
・・・Ｃ８と流した液を直接充填塔Ｃ１に戻すのではな
く、充填塔Ｃ８の末端から充填塔Ｃ１の頂部に戻る途中
に三方弁Ｇ８を用いて液を該循環ライン配管Ｊ側に流す
ようにし、この循環ライン配管を通した液を溶離液分配
管Ｄに合流させて充填塔Ｃ１の頂部に流し、しかもこの
循環ライン配管Ｊに流す三方弁Ｇ（Ｇ１〜Ｇ８）を各充
填塔間に各々設けて、上記した第１区画〜第４区画が一
定時間毎に下流側の充填塔に移行することに合わせて、
この三方弁Ｇによる流路切換えも移行させるようにした
装置であることを特徴としている。Example 2 In this example shown in FIG. 2, an independent circulation line branched from the piping of the packed tower group C instead of providing a circulation pump in the system of the packed tower group C shown in FIG. A pipe J and a circulating pump P11 on the way are provided, and for example, C2,.
... The three-way valve G8 is used to flow the liquid to the circulation line piping J on the way from the end of the packed tower C8 to the top of the packed tower C1, instead of directly returning the liquid flowing with C8 to the packed tower C1. The three-way valve G (G1 to G8) which flows through the circulation line pipe to the eluent distribution pipe D to flow to the top of the packed tower C1 and to flow through the circulation line pipe J is connected between the packed towers. In accordance with the above-mentioned first section to fourth section being shifted to the downstream packed tower at regular intervals,
The device is characterized in that the flow path switching by the three-way valve G is also shifted.
【００３１】そしてこの装置において、エクストラクト
液の抜き出しのために実施例１と同様に合流管Ｅの下流
に往復動型のポンプＰ４を設け、ラフィネート液抜き出
しのために実施例１と同様に合流管Ｒの下流に背圧弁Ａ
９を設けた。In this apparatus, a reciprocating pump P4 is provided downstream of the merging pipe E in the same manner as in the first embodiment for extracting the extract liquid, and the same as in the first embodiment for extracting the raffinate liquid. Back pressure valve A downstream of pipe R
9 were provided.
【００３２】このような装置においても、実施例１と同
様の効果を得ることができる。In such an apparatus, the same effects as in the first embodiment can be obtained.
【００３３】また本例の装置においては、第４区画の末
端からの液を循環ライン配管Ｊに液を流してから第１区
画の頂部に供給するので、循環系の各単位充填塔に対す
る液の流れは第１図の構成と全く同じに得ることができ
る上に、循環ポンプＰ１１に流れる液は常に第４区画末
端からの液となり、該循環ポンプＰ１１の流量を変更し
たり粘度の変化に対応する制御を行なうことが不要とな
る利点もある。In the apparatus of the present embodiment, the liquid from the end of the fourth section is supplied to the top of the first section after flowing the liquid through the circulation line piping J. The flow can be obtained in exactly the same manner as in the configuration of FIG. 1, and the liquid flowing to the circulation pump P11 always becomes the liquid from the end of the fourth section, and the flow rate of the circulation pump P11 can be changed or the viscosity can be changed. There is also an advantage that it is not necessary to perform such control.
【図１】第１図は、本発明の実施例１に用いた装置のフ
ローを示す説明図である。FIG. 1 is an explanatory diagram showing a flow of an apparatus used in a first embodiment of the present invention.
【図２】第２図は、本発明の実施例２に用いた装置のフ
ローを示す説明図である。FIG. 2 is an explanatory diagram showing a flow of an apparatus used in a second embodiment of the present invention.
【図３】第３図は、比較例に用いた装置のフローを示す
説明図である。FIG. 3 is an explanatory diagram showing a flow of an apparatus used in a comparative example.
Ｃ：充填塔 Ｆ１〜Ｆ８：原液供給弁 Ｄ１〜Ｄ８：溶離液供給弁 Ａ１〜Ａ８：ラフィネート液抜き出し弁 Ａ９：背圧弁 Ｂ１〜Ｂ８：エクストラクト液抜き出し弁 Ｐ１：循環ポンプ Ｐ２：溶離液供給ポンプ Ｐ３：原液供給ポンプ Ｐ４：エクストラクト液抜き出しポンプ Ｐ５：ラフィネート液抜き出しポンプ（系内圧を一定に
保つ自動制御付き） Ｈ：配管 Ｊ：循環ライン配管 Ｇ１〜Ｇ８：三方弁C: packed tower F1 to F8: stock solution supply valve D1 to D8: eluate supply valve A1 to A8: raffinate liquid extraction valve A9: back pressure valve B1 to B8: extract liquid extraction valve P1: circulation pump P2: eluent supply pump P3: Stock solution supply pump P4: Extract liquid extraction pump P5: Raffinate liquid extraction pump (with automatic control to keep the system internal pressure constant) H: Piping J: Circulation line piping G1 to G8: Three-way valve
フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) B01D 15/00 - 15/08 G01N 30/32 G01N 30/44 Continuation of the front page (58) Field surveyed (Int.Cl. 6 , DB name) B01D 15/00-15/08 G01N 30/32 G01N 30/44
Claims (5)
塔を無端直列に連結した系と、これらの単位充填塔のい
ずれかを選択して原液を供給する原液供給手段と、他の
いずれかの単位充填塔を選択して溶離液を供給する溶離
液供給手段と、いずれかの単位充填塔を選択してラフィ
ネート液を上記系外に抜き出す第１の液抜き出し手段
と、他のいずれかの単位充填塔を選択してエクストラク
ト液を系外に抜き出す第２の液抜き出し手段と、系内に
おける上記液の供給及び抜き出しの位置関係を相互に維
持して、これらの位置を系内の液流れ方向の下流側に順
次移行させる切換制御手段と、を備えた擬似移動層式ク
ロマト分離装置において、上記第１の液抜き出し手段又
は第２の液抜き出し手段のいずれか一方には抜き出し液
の流量をコントロールする流量制御手段を設けると共
に、これらの第１の液抜き出し手段又は第２の液抜き出
し手段のいずれか他方には、抜き出し上流側に予め定め
た一定圧の背圧を与える背圧付与手段を設けたことを特
徴とする擬似移動層式クロマト分離装置。1. A system in which a plurality of unit packed towers filled with an adsorbent are connected in an endless series, a stock solution supply means for selecting one of these unit packed towers and supplying a stock solution, An eluent supply means for selecting one of the unit packed towers and supplying an eluent; a first liquid extracting means for selecting one of the unit packed towers and extracting a raffinate solution out of the system; The second liquid extracting means for selecting the unit packed tower of (1) and extracting the extract liquid out of the system and the positional relationship between the supply and extraction of the liquid in the system are maintained mutually, and these positions are adjusted in the system. And a switching control means for sequentially shifting the liquid to the downstream side in the liquid flow direction, wherein either one of the first liquid extracting means or the second liquid extracting means has the extracted liquid. Control flow rate And a back pressure applying means for applying a predetermined constant pressure back pressure to the upstream side of the first liquid extracting means or the second liquid extracting means. A simulated moving bed type chromatographic separation apparatus, characterized in that:
特定成分に対して選択的吸着能力を有する吸着剤を充填
した多数の単位充填塔を、配管で直列に連結すると共
に、最後部の単位充填塔と最前部の単位充填塔をも配管
で連結することによって無端に連結した充填塔群を形成
し、該充填塔群を上流側から下流側に向かって第１区
画、第２区画、第３区画、第４区画に区画し、第１区画
の最前列に位置する単位充填塔の入口から溶離液を供給
弁を介して供給すると共に、第３区画の最前列に位置す
る単位充填塔の入口から原液を供給弁を介して供給し、
かつ第３区画の最後列に位置する単位充填塔の出口から
被吸着成分の少ないラフィネート液を抜き出し弁を介し
て抜き出すと共に、第１区画の最後列に位置する単位充
填塔の出口から被吸着成分の含有量の多いエクストラク
ト液を抜き出し弁を介して抜き出し、これらの溶離液の
供給位置、原液の供給位置、ラフィネート液の抜き出し
位置、エクストラクト液の抜き出し位置を、上記原液中
の成分の吸着剤に対する吸着領域の移行に伴って下流側
に繰り下げるように操作される擬似移動層式クロマト分
離装置において、ラフィネート液の抜き出し弁又はエク
ストラクト液の抜き出し弁のいずれか一方の配管に抜き
出し液の流量をコントロールする流量制御手段を設ける
と共に、ラフィネート液の抜き出し弁又はエクストラク
ト液の抜き出し弁のいずれか他方の配管には抜き出し弁
側に予め定めた一定圧の背圧を与える背圧付与手段を設
けたことを特徴とする擬似移動層式クロマト分離装置。2. A plurality of unit packed towers filled with an adsorbent having a selective adsorption capacity for a specific component of two or more components contained in a stock solution are connected in series by piping, A unit packed tower and a unit packed tower at the forefront are also connected by piping to form a packed tower group connected endlessly, and the packed tower group is divided into a first section and a second section from the upstream side to the downstream side. , A third section and a fourth section, the eluent is supplied via a supply valve from the inlet of the unit packed tower located in the front row of the first section, and the unit packing located in the front row of the third section. Undiluted solution is supplied from the inlet of the tower through a supply valve,
A raffinate solution containing a small amount of the component to be adsorbed is withdrawn from the outlet of the unit packed tower located in the last row of the third section through the extraction valve. The extract liquid having a high content of is extracted through the extraction valve, and the supply position of these eluents, the supply position of the stock solution, the extraction position of the raffinate solution, and the extraction position of the extract solution are determined by the adsorption of the components in the stock solution. In a simulated moving bed type chromatographic separation apparatus that is operated so as to be moved to the downstream side in accordance with the shift of the adsorption region for the agent, the flow rate of the extracted liquid is supplied to one of the pipes of the raffinate liquid extraction valve and the extract liquid extraction valve. And a flow control means for controlling the flow rate, and a raffinate liquid extraction valve or an extract liquid extraction valve Simulated moving bed chromatographic separator, characterized in that a back pressure applying means for applying a back pressure of a predetermined constant pressure on the withdrawal valve side to the other of the pipes.
には、ラフィネート抜き出し弁を介設したラフィネート
液抜き出し用配管と、エクストラクト抜き出し弁を介設
したエクストラクト液抜き出し用配管とがそれぞれ連結
されていると共に、各ラフィネート液抜き出し用配管は
共通のラフィネート液抜き出し用合流管に接続され、各
エクストラクト液抜き出し用配管は共通のエクストラク
ト液抜き出し用合流管に接続され、上記流量制御手段及
び背圧付与手段はこれらの合流管に設けられていること
を特徴とする擬似移動層式クロマト分離装置。3. The unit packing tower according to claim 1, wherein each unit packed column is provided with a raffinate liquid extracting pipe provided with a raffinate extracting valve and an extract liquid extracting pipe provided with an extract extracting valve. While connected, each raffinate liquid extracting pipe is connected to a common raffinate liquid extracting merging pipe, and each extract liquid extracting pipe is connected to a common extract liquid extracting merging pipe. And a simulated moving bed type chromatographic separation apparatus, wherein a back pressure applying means is provided in these confluent pipes.
圧付与手段が、背圧弁、逃がし弁、安全弁、ニードル
弁、オリフィス、抵抗管のいずれかであることを特徴と
する擬似移動層式クロマト分離装置。4. The simulated moving bed type according to claim 1, wherein the back pressure applying means is any one of a back pressure valve, a relief valve, a safety valve, a needle valve, an orifice, and a resistance pipe. Chromatographic separation equipment.
量制御手段が、流量制御可能のポンプであることを特徴
とする擬似移動層式クロマト分離装置。5. The simulated moving bed type chromatographic separation apparatus according to claim 1, wherein the flow rate control means is a pump capable of controlling the flow rate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3101643A JP2962589B2 (en) | 1991-05-07 | 1991-05-07 | Simulated moving bed chromatographic separator |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3101643A JP2962589B2 (en) | 1991-05-07 | 1991-05-07 | Simulated moving bed chromatographic separator |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04334503A JPH04334503A (en) | 1992-11-20 |
| JP2962589B2 true JP2962589B2 (en) | 1999-10-12 |
Family
ID=14306061
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3101643A Expired - Lifetime JP2962589B2 (en) | 1991-05-07 | 1991-05-07 | Simulated moving bed chromatographic separator |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2962589B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7488420B2 (en) | 2004-04-05 | 2009-02-10 | Organo Corporation | Chromatographic separator |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2785196B1 (en) * | 1998-10-29 | 2000-12-15 | Inst Francais Du Petrole | METHOD AND DEVICE FOR SEPARATION WITH VARIABLE LENGTH CHROMATOGRAPHIC AREAS |
| JP4587583B2 (en) * | 2000-03-10 | 2010-11-24 | 日本錬水株式会社 | Control method for chromatographic separation |
| JP4632327B2 (en) * | 2000-05-26 | 2011-02-16 | オルガノ株式会社 | Chromatographic separation device |
-
1991
- 1991-05-07 JP JP3101643A patent/JP2962589B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7488420B2 (en) | 2004-04-05 | 2009-02-10 | Organo Corporation | Chromatographic separator |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04334503A (en) | 1992-11-20 |
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