JPH04131761A - Liquid chromato-separation device of pseudo-moving floor type - Google Patents
Liquid chromato-separation device of pseudo-moving floor typeInfo
- Publication number
- JPH04131761A JPH04131761A JP2253944A JP25394490A JPH04131761A JP H04131761 A JPH04131761 A JP H04131761A JP 2253944 A JP2253944 A JP 2253944A JP 25394490 A JP25394490 A JP 25394490A JP H04131761 A JPH04131761 A JP H04131761A
- Authority
- JP
- Japan
- Prior art keywords
- zone
- pump
- circulation pump
- fluid
- eluent
- 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.)
- Granted
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 27
- 238000000926 separation method Methods 0.000 title claims abstract description 18
- 239000012530 fluid Substances 0.000 claims description 49
- 239000003480 eluent Substances 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 18
- 238000000746 purification Methods 0.000 claims description 17
- WSWCOQWTEOXDQX-MQQKCMAXSA-M (E,E)-sorbate Chemical compound C\C=C\C=C\C([O-])=O WSWCOQWTEOXDQX-MQQKCMAXSA-M 0.000 claims description 16
- 229940075554 sorbate Drugs 0.000 claims description 16
- 238000003795 desorption Methods 0.000 claims description 14
- 238000004811 liquid chromatography Methods 0.000 claims description 9
- 239000002594 sorbent Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- 230000000704 physical effect Effects 0.000 abstract description 7
- 238000007670 refining Methods 0.000 abstract 2
- 238000010586 diagram Methods 0.000 description 10
- 239000000945 filler Substances 0.000 description 9
- 238000000605 extraction Methods 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000012856 packing Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000005484 gravity Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、循環ポンプの数が少ないにもかかわらず、制
御機構の簡単な擬似移動床式液体クロマト分離装置に関
するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a simulated moving bed liquid chromatography separation apparatus with a simple control mechanism despite the small number of circulation pumps.
第６図は、従来の移動床による２成分分離の概念図であ
る。充填剤（固体収着剤）との親和力の強い成分Ａ（収
着質）と、充填剤との親和力の弱い成分Ｂ（非収着りと
を分離する場合、充填剤の詰まったカラム（充填床）内
の成分Ａと成分Ｂとの移動速度を、それぞれＶａ、 Ｖ
ｂとする。第６図に示すように、この中間の速度ｖｓで
充填剤を流体の流れ方向と逆方向に移動させると、成分
ＢはｖｂνＳの速度で流体移動方向に、成分ＡはＶｓ−
Ｖａの速度で充填剤移動方向にそれぞれ移動するから、
Ａ、Ｂの２成分の連続分離が可能となる。これは移動床
式としてよく知られている。FIG. 6 is a conceptual diagram of two-component separation using a conventional moving bed. When separating component A (sorbate), which has a strong affinity with the filler (solid sorbent), and component B (non-sorbent), which has a weak affinity with the filler, a column packed with the filler (packed The moving speeds of component A and component B in the floor) are Va and V, respectively.
b. As shown in FIG. 6, when the filler is moved in the direction opposite to the fluid flow direction at this intermediate speed vs, component B moves in the fluid flow direction at a speed vbνS, and component A moves Vs-
Since each moves in the filler movement direction at a speed of Va,
Continuous separation of the two components A and B becomes possible. This is commonly known as a moving bed type.
しかし、充填剤を実際に移動させることは、充填剤の摩
耗、空隙率の変化等を起こすので困難である。However, actually moving the filler is difficult because it causes wear of the filler, changes in porosity, and the like.
擬似移動床式では、１本のカラムを数本ないし十数本に
分割し、それぞれのカラムの入口、出口を一定周期で液
流れ方間に移動させることにより、実際に充填剤を移動
させることなしに、上述の機能を達成できるので、移動
床式の欠点を取り除き２成分（又は２成分とみなせる多
成分）の連続分離が可能になる。In the simulated moving bed system, one column is divided into several to ten or more columns, and the inlet and outlet of each column are moved in the direction of liquid flow at regular intervals to actually move the packing material. Since the above-mentioned functions can be achieved without using a moving bed system, continuous separation of two components (or multiple components that can be considered as two components) is made possible by eliminating the drawbacks of the moving bed method.
擬似移動床は、第７図に示すように、通常４つの帯域（
ゾーン）からなっている。一次精製帯域（ゾーン１）は
充填材との親和力の弱い成分Ｂ（非収着りを回収し溶離
液（脱着側流体）を再生するために、咬着帯域（ゾーン
２）は充填材との親和力の強い成分Ａ（収着質）と成分
Ｂとを分離しラフィ７−ト（非収着賞に富む流体）とし
て成分Ｂを回収するために、二次精製帯域（ゾーン３）
は成分Ｂを脱着させ成分Ａを精製するために、脱着帯域
（ゾーン４）は精製された成分Ａを脱着させエクストラ
クト（収着質に富む流体）として回収するために設けら
れている。As shown in Fig. 7, the pseudo moving bed usually has four bands (
zone). The primary purification zone (Zone 1) is used to collect component B (non-sorbed), which has a weak affinity with the filler, and to regenerate the eluent (desorption fluid). A secondary purification zone (Zone 3) is used to separate component A (sorbate) with strong affinity and component B and recover component B as raffite (fluid rich in non-sorption properties).
is provided to desorb component B and purify component A, and a desorption zone (zone 4) is provided to desorb purified component A and recover it as an extract (sorbate-rich fluid).
従来、擬似移動床としては、第８図に示すものが知られ
ている。１１〜２２は固体収着剤が充填されている単位
充填床で、これらの単位充填床の前端と後端とが流路で
連結されて無端状になっている。充填床内には循環ポン
プ３１により流体が一方向に循環し、この循環している
流体に原料液ポンプ４１により原料液を、溶離液ポンプ
４２により溶＃１液を導入し、同時に、充填床から非収
着譬に富む流体（ラフィネート）を流量弁４４を介して
抜き出すとともに、収着質に富む流体（エクストラクト
）をエクストラクトポンプ４３により抜き出す。Conventionally, as a pseudo moving floor, one shown in FIG. 8 is known. Unit packed beds 11 to 22 are filled with a solid sorbent, and the front and rear ends of these unit packed beds are connected by a flow path to form an endless shape. A fluid is circulated in one direction in the packed bed by a circulation pump 31, and a raw material liquid is introduced into the circulating fluid by a raw material liquid pump 41, and solution #1 is introduced by an eluent pump 42, and at the same time, the fluid is introduced into the packed bed. A fluid rich in non-sorbing substances (raffinate) is extracted from the fluid via a flow valve 44, and a fluid rich in sorbing substances (extract) is extracted by an extract pump 43.
そして、充填床内に導入され、又は充填床から抜き出さ
れる上記の流体の導入口及び抜出口を、循環している流
体の流れ方向に沿って交互に配置し、かつ、充填床を循
環している流体の流れ方向に充填床の導入口及び抜出口
の位置を間欠的に移動させることができるように構成さ
れている。ｖＦ〜νＦｌｉは原料液の供給を切り替える
ための三方電磁弁、ＶＤ＋”−ＶＤ＋ｚは溶＃液の供給
を切り替えるための三方電磁弁、ＶＲ＋〜ＶＪｉはラフ
ィネートの抜出しを切り替えるための三方電磁弁、ＶＥ
、〜ＶＥ＋ｚはエクストラクトの抜出しを切り替えるた
めの三方を磁弁である。The inlet and outlet for the above-mentioned fluid introduced into or extracted from the packed bed are arranged alternately along the flow direction of the circulating fluid, and the fluid is circulated through the packed bed. The structure is such that the positions of the inlet and the outlet of the packed bed can be moved intermittently in the flow direction of the fluid. vF~νFli are three-way solenoid valves for switching the supply of raw material liquid, VD+"-VD+z are three-way solenoid valves for switching the supply of solution #VR+~VJi are three-way solenoid valves for switching raffinate extraction, VE
, ~VE+z are three-way magnetic valves for switching extract extraction.
また、特開昭５５−７０３３６号公報には、第９図に示
すように、第８図に示す構成において循環ラインに１台
の循環ポンプを設ける代りに、単位充填床間の２個所以
上に複数台の定量ポンプ５１．５２．５３を設置し、−
時に１個所のポンプだけが作動するように、これらのポ
ンプを順次切替作動させるようにした擬似移動床が記載
されている。Furthermore, as shown in FIG. 9, JP-A-55-70336 discloses that instead of providing one circulation pump in the circulation line in the configuration shown in FIG. Install multiple metering pumps 51, 52, 53, -
A pseudo-moving bed is described in which the pumps are switched in sequence so that only one pump is in operation at a time.
〔発明が解決しようとする課題］
第８図に示す従来の擬似移動床では、循環ポンプ３１の
位置が一定であるので、周期的に循環ポンプ３１の吐出
流量を変化させなければならない。[Problems to be Solved by the Invention] In the conventional pseudo moving bed shown in FIG. 8, the position of the circulation pump 31 is constant, so the discharge flow rate of the circulation pump 31 must be changed periodically.
この循環流量が設定値からずれると、擬似移動床の分離
効率が大きく低下するので、この流量は精度良く制御す
ることが必要である。一方、循環ポンプに流入する流体
の組成も逐次変化するので、それにつれて流体の比重、
粘性等の物性も変化する。If this circulating flow rate deviates from the set value, the separation efficiency of the simulated moving bed will drop significantly, so it is necessary to control this flow rate with high precision. On the other hand, since the composition of the fluid flowing into the circulation pump changes sequentially, the specific gravity of the fluid changes accordingly.
Physical properties such as viscosity also change.
このような物性の変化及び設定値の変更に合わせて、プ
ログラム制御機器により流量を自動的に制御することは
、高価な制Ｗｌｌ器を必要とするとともに、通常の往復
動式定量ポンプで安定した流量が確保しにくい欠点があ
る。Automatically controlling the flow rate using a program-controlled device in response to changes in physical properties and set values requires an expensive controller and is not stable with a regular reciprocating metering pump. The disadvantage is that it is difficult to secure a sufficient flow rate.
また、特開昭５５−７０３３６号公報に記載された艦領
移動床においては、運転中に循環ポンプ（定量ポンプ５
１．５２．５３）の流量を変化させないようにしている
ので、制御機構はきわめて簡単である。In addition, in the ship's mobile bed described in Japanese Patent Application Laid-Open No. 55-70336, a circulation pump (metering pump 5) is used during operation.
1.52.53), the control mechanism is extremely simple.
しかし、循環ポンプ（定量ポンプ５１．５２．５３）に
流入する流体の組成も逐次変化するので、それにつれて
流体の比重、粘性等の物性も変化する。特に楯の分離等
で、原料の粘変が大きいときは、その変化が激しく、通
常の往復動式定量ポンプで安定した流量が確保しにくい
欠点がある。However, since the composition of the fluid flowing into the circulation pump (metering pump 51, 52, 53) changes sequentially, the physical properties of the fluid, such as specific gravity and viscosity, also change accordingly. In particular, when the viscosity of the raw material changes significantly due to separation of shields, etc., the change is drastic, making it difficult to secure a stable flow rate with a regular reciprocating metering pump.
本発明は上記の諸点に鑑みなされたもので、循環ポンプ
が常に一定の位置にくるように、充填床を１個ずつずら
して切り替えて４つの帯域（ゾーン）を形成し、循環ポ
ンプに導入される液の物性変化が小さくなるように構成
することにより、通常の往復動式定量ポンプで、安定し
た運転を行うことができる擬イ以移動床弐液体クロマト
分離装置を提供することを目的とするものである。The present invention was made in view of the above points, and in order to keep the circulation pump at a constant position, the packed beds are shifted and switched one by one to form four zones, which are introduced into the circulation pump. The purpose of the present invention is to provide a moving bed liquid chromatography separation device that can be operated stably using a normal reciprocating metering pump by configuring it so that changes in the physical properties of the liquid are minimized. It is something.
（課題を解決するための手段及び作用）上記の目的を達
成するために、本発明の擬領移動床弐液体りロマト分Ｈ
装置は、第１Ｖを参＠とで説明すれば、固体収着剤が充
填されていて、直列に配列されている４個以上の単位充
填床１１〜２２からなっており、これらの単位充填床の
前端と後端とが流路で連結されて無端状になっている充
填床内に流体を一方向に循環させ、この循環している流
体に原料液及び溶離液を導入し、同時に、単位充填床か
ら非収着質に富む流体及び収着質に富む流体を抜き出し
く充填床内に導入され、又はこれから抜き出される上記
４種の流体を以下の説明では側流と称することもある）
、充填床内に導入され又は充填床から抜き出される上記
の流体の導入口及び抜出口（以下、これらを側流口と称
することがある）を、循環している流体の流れ方向に沿
って交互に配置し、かつ、充填床を循環している流体の
流れ方向に充填床の導入口及び抜出口の位置を間欠的に
移動させるように構成されている擬似移動床式液体クロ
マト分Ｍ装胃において、１台の循環ポンプ４６を設け、
この循環ポンプ４６が常に一定の位置にくるように流路
を切り替えるための１を磁弁を配置したことを特徴とし
ている。(Means and effects for solving the problem) In order to achieve the above object, the pseudo-liquid moving bed liquid chromatographic fraction H of the present invention
The device consists of four or more unit packed beds 11 to 22 filled with a solid sorbent and arranged in series, if the first V is referred to as @. Fluid is circulated in one direction in an endless packed bed whose front end and rear end are connected by a flow path, and the raw material liquid and eluent are introduced into the circulating fluid, and at the same time, the unit The above-mentioned four types of fluids introduced into or extracted from the packed bed to extract non-sorbate-rich fluids and sorbate-rich fluids from the packed bed may also be referred to as side streams in the following description.
, the inlet and outlet for the above-mentioned fluid introduced into or extracted from the packed bed (hereinafter, these may be referred to as side flow ports) along the flow direction of the circulating fluid. A pseudo moving bed liquid chromatography separation device configured to alternately arrange the inlet and outlet ports of the packed bed intermittently in the flow direction of the fluid circulating through the packed bed. In the stomach, one circulation pump 46 is provided,
A feature is that a magnetic valve 1 is arranged to switch the flow path so that the circulation pump 46 is always at a constant position.
そして、上記の「一定の位置」は、一次精製帯域（ゾー
ン１）と脱着帯域（ゾーン４）との間であることが望ま
しい。The above-mentioned "certain position" is preferably between the primary purification zone (Zone 1) and the desorption zone (Zone 4).
また、循環ポンプ４６の背圧を、？８離液ポンプと背圧
弁とにより、又は第５図に示すように、溶離液ヘンドタ
ンクにより制御できるように、循環ポンプ４６の入口側
に溶離液ポンプ４７及び背圧弁４８を、又は溶離液ヘッ
ドタンク４９を接続する。Also, what is the back pressure of the circulation pump 46? 8. An eluent pump 47 and a back pressure valve 48 are installed on the inlet side of the circulation pump 46, or an eluent head tank so that the eluent pump 47 and a back pressure valve 48 can be controlled by a syneresis pump and a back pressure valve, or by an eluent head tank as shown in FIG. Connect 49.
擬似移動床では、同時に４個の側流口が作動し、充填床
はその機能上、これらの側流口により４個の帯域（ゾー
ン）、すなわち、原料液導入口から非収着質に富む流体
（ラフィネート）の抜出口までの間を占める吸着帯域（
ゾーン２）、非収着質に富む流体の抜出口から脱着剤流
体（７＠ ｉＩｆ液）導入口までの間を占める一次精製
帯域（ゾーン１）、脱着側流体導入口から収着質に富む
流体（エクスＩ・ラクト）の抜出口までの間を占める脱
着帯域（ゾーン４）、収着質に富む流体の抜出口から原
料液導入口までの間を占める二次精製帯域（ゾーン３）
の４個の帯域（ゾーン）からなっている。In the simulated moving bed, four side ports are operated at the same time, and the packed bed is functionally divided into four zones (zones) by these side ports, i.e., non-sorbate-rich from the raw material inlet. Adsorption zone (
Zone 2), the primary purification zone (Zone 1) that occupies the area from the non-sorbate-rich fluid outlet to the desorbent fluid (7@iIf fluid) inlet, and the sorbate-rich zone from the desorption side fluid inlet. A desorption zone (Zone 4) that occupies the area between the fluid (Ex-I/Lact) outlet and a secondary purification zone (Zone 3) that occupies the area from the sorbate-rich fluid outlet to the raw material liquid inlet.
It consists of four bands (zones).
〔実施例］
以下、図面を参照して本発明の好適な実施例を詳細に説
明する。ただしこの実施例に記載されている構成機器の
形状、その相対配置などは、とくに特定的な記載がない
限りは、本発明の範囲をそれらのみに限定する趣旨のも
のではなく、単なる説明例にすぎない。[Embodiments] Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings. However, unless there is a specific description, the shapes of the components described in this example, their relative positions, etc. are not intended to limit the scope of the present invention to these, but are merely illustrative examples. Only.
第１図は、−例として１２個の単位充填床１１〜２２を
備えた擬（以移動床弐液体クロマト分離装置を示してい
る。単位充填床間は循環溝ｇＩ６０１〜６１２で連絡さ
れている。原料液は原料液ポンプ４１、原料液導管８０
７及びこれに連絡している原料液導入分岐管４０１〜４
１２を経て各単位充填床に導入される。FIG. 1 shows, as an example, a pseudo-moving bed liquid chromatography separation apparatus equipped with 12 unit packed beds 11 to 22. The unit packed beds are connected by circulation grooves gI601 to 612. The raw material liquid is supplied through the raw material liquid pump 41 and the raw material liquid conduit 80.
7 and raw material liquid introduction branch pipes 401 to 4 connected thereto.
12 into each unit packed bed.
原料液導入分岐管４０１〜４１２には三方電磁弁ＶＦ、
〜ＶＦ、、が設けられている。脱着剤流体（溶離ｆｉ）
は溶離液ポンプ４７、溶離液導管８０８、循環ポンプ４
６、循環導管８１０、溶Ｒ液導入分岐管５０１〜５１２
を経て各単位充填床に導入される。この分岐管５０１〜
５１２にも三方電磁弁ＶＤ、〜ＶＤ＋ｚが設けられてい
る。The raw material liquid introduction branch pipes 401 to 412 have three-way solenoid valves VF,
~VF, , are provided. Desorbent fluid (elution fi)
The eluent pump 47, the eluent conduit 808, and the circulation pump 4
6. Circulation conduit 810, solution R liquid introduction branch pipes 501 to 512
It is then introduced into each unit packed bed. This branch pipe 501~
512 is also provided with three-way solenoid valves VD, ~VD+z.
収着質に富む流体（エクストラクト）は、エクストラク
ト抜出分岐管２０１〜２１２、エクストラクト導管８０
５、エクストラクトポンプ４３を経て各単位充填床から
抜き出される。これらの分岐管２０１〜２１２には三方
電磁弁ＶＥ、〜ＶＥ１２が設けられている。一方、非収
着賞に富む流体（ラフィネート）は、ラフィネート抜出
分岐管３０１〜３１２、ラフィネート導管８０６、ラフ
ィネートポンプ４５を経て各単位充填床から抜き出され
る。これらの分岐管３０１〜３１２にも三方１１磁弁Ｖ
Ｒ，〜ＶＲ１ｔが設けられている。The sorbate-rich fluid (extract) is extracted through extract extraction branch pipes 201 to 212 and extract conduit 80.
5. Extracted from each unit packed bed via the extract pump 43. These branch pipes 201-212 are provided with three-way solenoid valves VE, -VE12. On the other hand, the non-sorption rich fluid (raffinate) is extracted from each unit packed bed via the raffinate extraction branch pipes 301 to 312, the raffinate conduit 806, and the raffinate pump 45. These branch pipes 301 to 312 also have three-way 11 magnetic valves V.
R, to VRlt are provided.
エクストラクト抜出分岐管２０１〜２１２とラフィネー
ト抜出分岐管３０１〜２１２とをそれぞれ接続する導管
には、それぞれ三方電磁弁ＶＴ、〜ＶＴ、□が設けられ
、これらの三方電磁弁νＴ、〜ＶＴ、□の一方は、導管
９０１〜９１２を介して溶離液ポンプ４７が接続された
Ｗｉ環導管８１０に接続されている。The conduits connecting the extract extraction branch pipes 201 to 212 and the raffinate extraction branch pipes 301 to 212, respectively, are provided with three-way solenoid valves VT, ~VT, and □, and these three-way solenoid valves νT, ~VT , □ are connected to the Wi ring conduit 810 to which the eluent pump 47 is connected via conduits 901 to 912.
ラフィぶ一トボンブ４５、エクストラクトポンプ４３、
原料液ポンプ４１及び循環ポンプ４６は、いずれも流量
が設定値（一定）となるように制御される。また、循環
ポンプ４６の背圧が設定値（一定）となるように、溶離
液ポンプ４７及び背圧弁４８が制御される。Luffy Button Bomb 45, Extract Pump 43,
The raw material liquid pump 41 and the circulation pump 46 are both controlled so that their flow rates are at a set value (constant). Further, the eluent pump 47 and the back pressure valve 48 are controlled so that the back pressure of the circulation pump 46 becomes a set value (constant).
つぎに、本発明におけるｔｍ弁の開閉サイクルの一例に
ついて、単位充填床が１２本の場合について説明する。Next, an example of the opening/closing cycle of the tm valve in the present invention will be described in the case where there are 12 unit packed beds.
分離パターンは、一次精製帯域（ゾーン１）、吸着帯域
（ゾーン２）、二次精製帯域（ゾーン３）、脱着帯域（
ゾーン４）かいずれも３本ずつとなるＪ
単位充填床が１２本であるので、１２通りのステップが
行われることになる。−例として、ステップ１を第２図
に、ステップ２を第３図に、ステップ３を第４図に示す
、この場合の各電磁弁の開閉状態は第１表に示す通りで
ある。The separation pattern consists of a primary purification zone (Zone 1), an adsorption zone (Zone 2), a secondary purification zone (Zone 3), and a desorption zone (Zone 3).
Since there are 12 J unit packed beds (3 in each zone 4), 12 steps are performed. - As an example, step 1 is shown in FIG. 2, step 2 is shown in FIG. 3, and step 3 is shown in FIG. 4. In this case, the opening and closing states of each solenoid valve are as shown in Table 1.
第
表
第２図のステップ１において、原料液は充填床１７に供
給され、充填床１８．１９を循環する。In step 1 of Table 2, the raw liquid is fed to the packed bed 17 and circulated through the packed beds 18, 19.
この間に収着質に富む物質は充填剤に吸着され、非収看
質に富む流体が充填床１９からラフィネートとして抜き
出される。すなわち、充填床１７〜１９は吸着帯域（ゾ
ーン２）となる。During this time, the sorbate-rich material is adsorbed by the packing material, and the non-sorbate-rich fluid is withdrawn from the packed bed 19 as a raffinate. That is, the packed beds 17 to 19 become an adsorption zone (zone 2).
一方、溶離液を含む循環流体は充填床１１に供給され、
充填床１２．１３を循環する。この間に充填剤に吸着さ
れていた収着質は脱着し、収着質に富む流体が充填床１
３からエクストラクトとして抜き出される。すなわち、
充填床１１〜１３は脱着帯域（ゾーン４）となる。On the other hand, the circulating fluid containing the eluent is supplied to the packed bed 11,
Cycle through packed beds 12.13. During this time, the sorbate adsorbed by the packing material is desorbed, and the sorbate-rich fluid is transferred to the packed bed 1.
It is extracted as an extract from 3. That is,
Packed beds 11-13 become the desorption zone (zone 4).
充填床２０〜２２へは循環流体が循環され、この間に非
収着賞は充填剤に吸着され、収着質も非収着賞も含まな
い流体となり、充填床２２から抜き出される。すなわち
、充填床２０〜２２は一次精製帯域（ゾーンｌ）となる
。A circulating fluid is circulated through the packed beds 20 to 22, during which non-sorbed particles are adsorbed by the filler, resulting in a fluid containing neither sorbate nor non-sorbed particles, which is extracted from the packed bed 22. That is, the packed beds 20 to 22 become the primary purification zone (zone 1).
充填床１４〜１６へは循環流体が循環され、この間に充
填剤に吸着されていた非収着賞は脱着され、一方、収着
質は充填剤に吸着され精製される。Circulating fluid is circulated through the packed beds 14 to 16, during which non-sorbed substances adsorbed on the packing material are desorbed, while sorbates are adsorbed on the packing material and purified.
すなわち、充填床１４〜１６は二次精製帯域（ゾーン３
）となる。That is, packed beds 14-16 are in the secondary purification zone (Zone 3).
).
第３図のステップ２においては、ステップ１における状
態が充填床１本分左側にずれて切り替えられ、充填床１
２〜１４が脱着帯域（ゾーン４）、充填床１５〜１７が
二次精製帯域（ゾーン３）、充填床１８〜２０が吸着帯
域（ゾーン２）、充填床２）、２２．１１が一次精製帯
域（ゾーン１）となる。In step 2 of FIG. 3, the state in step 1 is shifted to the left by one packed bed, and the state in step 1 is shifted to the left by one packed bed.
2 to 14 are desorption zones (zone 4), packed beds 15 to 17 are secondary purification zones (zone 3), packed beds 18 to 20 are adsorption zones (zone 2), packed beds 2), and 22.11 is primary purification zones. band (Zone 1).
第４図のステップ３においては、ステップ２における状
態がさらに充填床１本分左側にずれて切り替えられ、充
填床１３〜１５が脱着帯域（ゾーン４）、充填床１６〜
１８が二次精製帯域（ゾーン３）、充填床１９〜２１が
吸着帯域（ゾーン２）、充填床２２．１１．１２が一次
精製帯域（ゾーン１）となる。In step 3 of FIG. 4, the state in step 2 is further shifted to the left by one packed bed, and packed beds 13 to 15 are in the desorption zone (zone 4), packed beds 16 to 15 are in the desorption zone (zone 4), and packed beds 16 to
18 is the secondary purification zone (Zone 3), packed beds 19 to 21 are the adsorption zone (Zone 2), and packed beds 22, 11, and 12 are the primary purification zone (Zone 1).
以下、図示していないが、充填床１本分づつ左側にずれ
て切り替えられ、ステップ１２まで行われ、これらの動
作が繰り返される。Thereafter, although not shown, the switching is shifted to the left by one packed bed at a time, and steps up to step 12 are performed, and these operations are repeated.
いずれのステップにおいても、循環ポンプ４６の吸引導
管は一次精製帯域（ゾーン１）の最終段充填床の出口に
接続され、循環ポンプ４６の吐出導管は脱着帯域（ゾー
ン４）の第１段充填床の入口に接続されることになる。In either step, the suction conduit of the circulation pump 46 is connected to the outlet of the last packed bed in the primary purification zone (Zone 1), and the discharge conduit of the circulation pump 46 is connected to the outlet of the first packed bed in the desorption zone (Zone 4). It will be connected to the entrance of
このため、循環ポンプ４６に導入される液の物性変化が
小さくなり、安定運転を行うことができる。特に、−次
精製帯域（ゾーン１）と脱着帯域（ゾーン４）との間は
、粘度が最も低くなり好適である。Therefore, changes in the physical properties of the liquid introduced into the circulation pump 46 are reduced, and stable operation can be performed. In particular, the viscosity is the lowest between the secondary purification zone (Zone 1) and the desorption zone (Zone 4), which is preferable.
なお、本発明においては、特開昭５５−７０３３６の装
置に比べて電磁弁の数が増えるが、ポンプの数は少なく
なり、を磁弁は定量ポンプに比べて安価なこと、及び制
御系が簡単なことから、全体の装置コストは低減される
。In addition, in the present invention, the number of solenoid valves is increased compared to the device of JP-A-55-70336, but the number of pumps is decreased. Due to its simplicity, the overall equipment cost is reduced.
第５図は本発明の装置の他の実施例を示している。本例
は循環導管８１０に溶離液ポンプ及び背圧弁を接続する
代りに、循環導管８１０に溶離液ヘッドタンク４９を接
続したものである。このタンク４９に常に一定深さとな
るように溶離液を供給する。他の構成、作用は第１図〜
第４図の場合と四棒である。FIG. 5 shows another embodiment of the device according to the invention. In this example, an eluent head tank 49 is connected to the circulation conduit 810 instead of an eluent pump and a back pressure valve connected to the circulation conduit 810. The eluent is supplied to this tank 49 so that it always has a constant depth. Other configurations and functions are shown in Figure 1~
In the case of Figure 4, there are four bars.
本発明は上記のように構成されているので、つぎのよう
な効果を奏する。Since the present invention is configured as described above, it has the following effects.
（１）運転中に循環ポンプの流量を変化させないように
しているので、制御機構がきわめて簡単となり、安価に
製作することができる。(1) Since the flow rate of the circulation pump is not changed during operation, the control mechanism is extremely simple and can be manufactured at low cost.
（２）循環ポンプが常に一定の位置にくるので、循環ポ
ンプに導入される液の物性変化が小さく、このため、通
常の往復動式定量ポンプで安定した流量を確保すること
ができる。特に、−次精製帯域（ゾーン１）と脱着帯域
（ゾーン４）との間の場合は、粘度が最も低く好適であ
る。(2) Since the circulation pump is always at a constant position, changes in the physical properties of the liquid introduced into the circulation pump are small, and therefore a stable flow rate can be ensured with a normal reciprocating metering pump. In particular, the zone between the secondary purification zone (Zone 1) and the desorption zone (Zone 4) is preferred because it has the lowest viscosity.
第１図は本発明の擬位移動床弐液体クロマト分離装置の
一実施例を示す概念説明図、第２図は第１図に示す装置
におけるステップ１の状態を示す概念説明図、第３図は
ステップ２の状態を示す概念説明図、第４図はステップ
３の状態を示す概念説明図、第５図は本発明の装置の他
の実施例を示す概念説明図、第６図は一般の移動床によ
る２成分分離の概念圀、第７図は擬似移動床式連続液体
クロマト分離装置の一般的な構成を示す説明図、第８図
及び第９図は従来の擬似移動床を示す概念説明図である
。
１１〜２２・・・充填床、３１・・・循環ポンプ、４１
・・・原料液ポンプ、４２・・・溶離液ポンプ、４３・
・・エクストラクトポンプ、４４・・・流量弁、４５・
・・ラフィふ一トポンプ、４６・・・循環ポンプ、４７
・・・溶離液ポンプ、４８・・・背圧弁、４９・・・ｉ
９ ’７Ｍ 液ヘツドタンク、５１．５２．５３・・・
定量ポンプ、ｖＦ１〜ｖＦ１２・・原料液用の三方を磁
弁、ＶＤ１〜ＶＤ、□・・・溶離液用の三方ｔｍ弁、Ｖ
Ｒ，〜ｖｌＬｔ・・・ラフィネート用の一方ｔｍ弁、Ｖ
Ｂ、−ＶＥ、２・・・エクストラクト用の三方電磁弁、
νＴ１〜ＶＴｌｔ・・・三方電磁弁、２０１〜２１２・
・・エクストラクト抜出分岐管、３０１〜３１２・・・
ラフィネート抜出分岐管、４０１〜４１２・・・原料液
導入分岐管、５０１〜５１２・・・溶離液導入分岐管、
６０１〜６１２・・・循環導管、８０５・・・エクスト
ラクト導管、８０６・・・ラフィネート導管、８０７・
・・原料液導管、８０８・・・溶離液導管、８１０・・
・循環導管、９０１〜９１２・・・導管出 願 人
川崎重工業株式会社FIG. 1 is a conceptual explanatory diagram showing an embodiment of the pseudomorphic moving bed liquid chromatography separation apparatus of the present invention, FIG. 2 is a conceptual explanatory diagram showing the state of step 1 in the apparatus shown in FIG. 1, and FIG. is a conceptual diagram showing the state of step 2, FIG. 4 is a conceptual diagram showing the state of step 3, FIG. 5 is a conceptual diagram showing another embodiment of the device of the present invention, and FIG. 6 is a general diagram Conceptual diagram of two-component separation using a moving bed. Figure 7 is an explanatory diagram showing the general configuration of a simulated moving bed type continuous liquid chromatography separation device. Figures 8 and 9 are conceptual explanations showing a conventional simulated moving bed. It is a diagram. 11-22... Packed bed, 31... Circulation pump, 41
... Raw material liquid pump, 42... Eluent pump, 43.
・・Extract pump, 44・・Flow rate valve, 45・
...Raffi fuito pump, 46...Circulation pump, 47
...Eluent pump, 48...Back pressure valve, 49...i
9 '7M Liquid head tank, 51.52.53...
Metering pump, vF1-vF12... three-way magnetic valve for raw material liquid, VD1-VD, □... three-way tm valve for eluent, V
R, ~vlLt... One-way tm valve for raffinate, V
B, -VE, 2... Three-way solenoid valve for extract,
νT1~VTlt...Three-way solenoid valve, 201~212.
...Extract extraction branch pipe, 301-312...
Raffinate extraction branch pipe, 401-412... Raw material liquid introduction branch pipe, 501-512... Eluent introduction branch pipe,
601-612... Circulation conduit, 805... Extract conduit, 806... Raffinate conduit, 807.
... Raw material liquid conduit, 808... Eluent conduit, 810...
・Circulation conduits, 901-912... Conduit applicant
Kawasaki Heavy Industries Co., Ltd.
Claims (1)
る４個以上の単位充填床（１１〜２２）からなっており
、これらの単位充填床の前端と後端とが流路で連結され
て無端状になっている充填床内に流体を一方向に循環さ
せ、この循環している流体に原料液及び溶離液を導入し
、同時に、単位充填床から非収着質に富む流体及び収着
質に富む流体を抜き出し、充填床内に導入され又は充填
床から抜き出される上記の流体の導入口及び抜出口を、
循環している流体の流れ方向に沿って交互に配置し、か
つ、充填床を循環している流体の流れ方向に充填床の導
入口及び抜出口の位置を間欠的に移動させるように構成
されている擬似移動床式液体クロマト分離装置において
、 １台の循環ポンプ（４６）を設け、この循環ポンプ（４
６）が常に一定の位置にくるように流路を切り替えるた
めの電磁弁を配置したことを特徴とする擬似移動床式液
体クロマト分離装置。 ２ 一定の位置が、一次精製帯域と脱着帯域との間であ
ることを特徴とする請求項１記載の擬似移動床式液体ク
ロマト分離装置。 ３ 循環ポンプ（４６）の背圧を、溶離液ポンプと背圧
弁とにより、又は溶離液ヘッドタンクにより制御できる
ように、循環ポンプ（４６）の入口側に溶離液ポンプ（
４７）及び背圧弁（４８）を、又は溶離液ヘッドタンク
（４９）を接続したことを特徴とする請求項１又は２記
載の擬似移動床式液体クロマト分離装置。[Scope of Claims] 1 Consists of four or more unit packed beds (11 to 22) filled with a solid sorbent and arranged in series, with front and rear ends of these unit packed beds A fluid is circulated in one direction in an endless packed bed in which the two are connected by a flow path, and a raw material liquid and an eluent are introduced into the circulating fluid. An inlet and an outlet for the above-mentioned fluids to be introduced into the packed bed or extracted from the packed bed for extracting the sessile-rich fluid and the sorbate-rich fluid,
The packed bed is arranged alternately along the flow direction of the circulating fluid, and the positions of the inlet and outlet of the packed bed are intermittently moved in the flow direction of the circulating fluid. In the simulated moving bed type liquid chromatography separation device, one circulation pump (46) is installed, and this circulation pump (46) is installed.
6) A pseudo moving bed type liquid chromatography separation device characterized in that a solenoid valve for switching a flow path is arranged so that 6) is always at a constant position. 2. The simulated moving bed liquid chromatography separation apparatus according to claim 1, wherein the fixed position is between the primary purification zone and the desorption zone. 3. An eluent pump (46) is installed on the inlet side of the circulation pump (46) so that the back pressure of the circulation pump (46) can be controlled by the eluent pump and the back pressure valve or by the eluent head tank.
47) and a back pressure valve (48), or an eluent head tank (49).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2253944A JPH0695090B2 (en) | 1990-09-21 | 1990-09-21 | Pseudo moving bed liquid chromatographic separation device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2253944A JPH0695090B2 (en) | 1990-09-21 | 1990-09-21 | Pseudo moving bed liquid chromatographic separation device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04131761A true JPH04131761A (en) | 1992-05-06 |
| JPH0695090B2 JPH0695090B2 (en) | 1994-11-24 |
Family
ID=17258164
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2253944A Expired - Lifetime JPH0695090B2 (en) | 1990-09-21 | 1990-09-21 | Pseudo moving bed liquid chromatographic separation device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0695090B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995023125A1 (en) * | 1994-02-25 | 1995-08-31 | Daicel Chemical Industries, Ltd. | Process for producing optically active mevalonolactone compound |
| JP2022500241A (en) * | 2018-11-14 | 2022-01-04 | 内蒙古伊泰煤基新材料研究院有限公司Inner Mongolia Yitai Coal−Based New Materials Research Institute Co., Ltd. | High-efficiency pseudo-moving floor equipment and high-efficiency pseudo-moving floor process |
Families Citing this family (1)
| 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 |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5570336A (en) * | 1978-11-22 | 1980-05-27 | Mitsubishi Chem Ind Ltd | Pseudomoving bed |
| JPS62190463U (en) * | 1986-05-26 | 1987-12-03 | ||
| JPS62199674U (en) * | 1986-06-11 | 1987-12-19 | ||
| JPS6483152A (en) * | 1987-09-25 | 1989-03-28 | Japan Spectroscopic Co | Recycling chromatograph |
| JPH01165953A (en) * | 1987-12-23 | 1989-06-29 | Hitachi Ltd | Liquid chromatograph |
| JPH0249159A (en) * | 1988-05-17 | 1990-02-19 | Mitsubishi Kasei Techno Engineers Kk | Chromatographic separation |
| JPH0264453A (en) * | 1988-08-30 | 1990-03-05 | Shimadzu Corp | Recycle liquid chromatography |
-
1990
- 1990-09-21 JP JP2253944A patent/JPH0695090B2/en not_active Expired - Lifetime
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5570336A (en) * | 1978-11-22 | 1980-05-27 | Mitsubishi Chem Ind Ltd | Pseudomoving bed |
| JPS62190463U (en) * | 1986-05-26 | 1987-12-03 | ||
| JPS62199674U (en) * | 1986-06-11 | 1987-12-19 | ||
| JPS6483152A (en) * | 1987-09-25 | 1989-03-28 | Japan Spectroscopic Co | Recycling chromatograph |
| JPH01165953A (en) * | 1987-12-23 | 1989-06-29 | Hitachi Ltd | Liquid chromatograph |
| JPH0249159A (en) * | 1988-05-17 | 1990-02-19 | Mitsubishi Kasei Techno Engineers Kk | Chromatographic separation |
| JPH0264453A (en) * | 1988-08-30 | 1990-03-05 | Shimadzu Corp | Recycle liquid chromatography |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995023125A1 (en) * | 1994-02-25 | 1995-08-31 | Daicel Chemical Industries, Ltd. | Process for producing optically active mevalonolactone compound |
| US5939552A (en) * | 1994-02-25 | 1999-08-17 | Daicel Chemical Industries, Ltd. | Process for preparing optically active mevalonolactone compounds |
| JP2022500241A (en) * | 2018-11-14 | 2022-01-04 | 内蒙古伊泰煤基新材料研究院有限公司Inner Mongolia Yitai Coal−Based New Materials Research Institute Co., Ltd. | High-efficiency pseudo-moving floor equipment and high-efficiency pseudo-moving floor process |
| US11980833B2 (en) | 2018-11-14 | 2024-05-14 | Inner Mongolia Yitai Coal-Based New Materials Research Institute Co., Ltd. | Efficient simulated moving bed device and efficient simulated moving bed process |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0695090B2 (en) | 1994-11-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR960010366B1 (en) | Method of choromatographic separation | |
| KR101164239B1 (en) | Improved simulated moving bed separation process and device | |
| US4923616A (en) | Method of separating chemical components in simulated moving bed | |
| JP5330499B2 (en) | Gradient elution multi-column separation method | |
| US4434051A (en) | Multiple valve apparatus for simulated moving bed adsorption processes | |
| US3323292A (en) | Apparatus for fractionating gaseous mixtures | |
| US6979402B1 (en) | Miniature actual moving bed assembly | |
| US3706812A (en) | Fluid-solid contacting apparatus | |
| JPH0229361B2 (en) | ||
| KR930000142A (en) | Separation method of plural components | |
| JP6013639B1 (en) | Chromatographic separation method and apparatus for separating multiple components into three or more fractions | |
| US3992175A (en) | Method of and device for chromatographic separation of fluid mixtures into fractions | |
| JPH04131761A (en) | Liquid chromato-separation device of pseudo-moving floor type | |
| JP3277575B2 (en) | Chromatographic separation method | |
| AU566829B2 (en) | Method for preventing compaction in sorbent beds | |
| JP4606092B2 (en) | Pseudo moving bed type chromatographic separation method and apparatus | |
| JP2740780B2 (en) | Simulated moving bed equipment | |
| KR101084628B1 (en) | Apparatus and method for improving the separation by simulated moving bed process with feed chromatographic column | |
| JPH0639205A (en) | Liquid chromatographic separator for three components | |
| JPH07106282B2 (en) | Method and apparatus for separating and purifying multi-component mixture | |
| KR101106004B1 (en) | A simulated moving bed separation apparatus and a separative method of a fluid using the same | |
| JPH0639206A (en) | Pseudo moving-bed liquid chromatographic separator | |
| JP2648366B2 (en) | Separation method using simulated moving bed | |
| US7022229B1 (en) | Adsorption separation system | |
| JP2965747B2 (en) | Multicomponent separation method and apparatus |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20071124 Year of fee payment: 13 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20081124 Year of fee payment: 14 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091124 Year of fee payment: 15 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091124 Year of fee payment: 15 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101124 Year of fee payment: 16 |
|
| EXPY | Cancellation because of completion of term |