JPH0716401A - Chromatographic separation - Google Patents
Chromatographic separationInfo
- Publication number
- JPH0716401A JPH0716401A JP32311691A JP32311691A JPH0716401A JP H0716401 A JPH0716401 A JP H0716401A JP 32311691 A JP32311691 A JP 32311691A JP 32311691 A JP32311691 A JP 32311691A JP H0716401 A JPH0716401 A JP H0716401A
- Authority
- JP
- Japan
- Prior art keywords
- section
- component
- packed
- packed column
- affinity
- 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
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、原液中に含まれる３以
上の成分に対して選択的な吸着能力を有する吸着剤を充
填した多数の充填塔を、直列かつ無端に連結した擬似移
動層式クロマト分離装置を用いた分離法に関するもので
あり、例えばマルトースとグルコースとフルクトースと
の分離、マルトトリオースとマルトースとグルコースと
の分離法等に関する。TECHNICAL FIELD The present invention relates to a simulated moving bed in which a large number of packed columns packed with an adsorbent having a selective adsorption capacity for three or more components contained in a stock solution are connected in series and endlessly. The present invention relates to a separation method using a chromatographic separation device, for example, a separation method between maltose, glucose and fructose, a separation method between maltotriose, maltose and glucose, and the like.
【０００２】[0002]
【従来の技術】従来、吸着剤を充填した充填塔に２成分
を含む液体を流してこれらの成分が富化された画分を分
離して回収するクロマト分離法は、固定床式、擬似移動
層式、流動層式として知られており、近時においては３
以上の成分を分離する目的で擬似移動層式のクロマト分
離法が注目され、既にいくつかの提案もされている。2. Description of the Related Art Conventionally, a chromatographic separation method in which a liquid containing two components is made to flow in a packed column filled with an adsorbent to separate and collect a fraction enriched in these components is a fixed bed type, a simulated moving type. It is known as a layered type or fluidized bed type, and in recent years it has been 3
For the purpose of separating the above components, a simulated moving bed type chromatographic separation method has been attracting attention and some proposals have already been made.
【０００３】このような擬似移動層式クロマト分離装置
を用いて多成分の分離を行なう方法としては、原料流体
中に含まれる３成分以上の成分に対する吸着能力に差が
ある吸着剤を充填した多数の充填塔を、１台ないし数台
の循環ポンプと共に、配管で無端直列に連結し、この充
填塔群に原料流体を流して上流側から下流側に向かっ
て、各成分の富化された状態が異なる第１区画、第２区
画、第３区画、第４区画を形成させて以下のａ，ｂの操
作を繰り返して行なうものが代表的に知られている。As a method for separating multiple components using such a simulated moving bed chromatographic separation device, a large number of adsorbents having different adsorption capacities with respect to three or more components contained in the raw material fluid are filled. The packed column of No. 1 is connected with one or several circulating pumps in an endless series by piping, and the raw material fluid is flowed through this packed column group to enrich each component from the upstream side to the downstream side. It is typically known that a first section, a second section, a third section, and a fourth section which are different from each other are formed and the following operations a and b are repeated.
【０００４】ａ： 第２区画と第３区画の間の遮断弁を
閉じ、第１区画の最前列の充填塔の入口から脱着剤を、
第３区画の最前列に位置する充填塔の入口から原料を供
給し、さらに第２区画の最後列に位置する充填塔の出口
から吸着剤に対する親和力が１番強くも弱くもない成分
Ｂが富化された画分を流出させる第１の工程 ｂ： 遮断弁を開き、充填層内の流体を循環しつつ、第
１区画の最前列の充填塔の入口から脱着剤を供給し、第
３区画の最後列の充填塔から吸着剤に対する親和力が弱
い成分Ａが富化された画分を、第１区画の最後列に位置
する充填塔の出口から吸着剤に対する親和力が強い成分
Ｃが富化された画分を流出させ、また脱着剤の供給位
置、各画分の流出位置を、ロータリー弁あるいは各塔に
付設した弁によって下流側に順次移動させる第２の工程A: The shutoff valve between the second and third compartments is closed, and the desorbent is introduced from the inlet of the packed column in the front row of the first compartment,
The raw material is supplied from the inlet of the packed column located in the front row of the third section, and the component B, which has neither strong nor weaker affinity for the adsorbent, is supplied from the outlet of the packed column located in the last row of the second section. First step of flowing out the converted fraction b: Opening the shut-off valve and circulating the fluid in the packed bed, while supplying the desorbent from the inlet of the packed column in the front row of the first section, the third section The fraction enriched with the component A having a weak affinity for the adsorbent from the packed column in the last row of the column is enriched with the component C having a strong affinity for the adsorbent from the outlet of the packed column located in the last row of the first section. The second step in which the desorbent supply position and the outflow position of each fraction are sequentially moved to the downstream side by a rotary valve or a valve attached to each tower.
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、前述し
た従来の多成分分離擬似移動層式クロマト分離装置の流
量制御は複雑であり、流量制御機器は高性能で高価な物
が必要であった。特に、小型で種々の用途に汎用的に使
え、制御が簡単で、安価な多成分分離擬似移動層式クロ
マト分離法が求められていた。However, the flow control of the above-mentioned conventional multi-component separation pseudo moving bed type chromatographic separation device is complicated, and the flow control device needs to be high performance and expensive. In particular, there has been a demand for a multi-component separation pseudo-moving bed chromatographic separation method that is small in size, versatile in various uses, easy to control, and inexpensive.
【０００６】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多成分分離擬似移動層式
クロマト分離法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。From the above viewpoints, the present inventor has conducted various studies and developed the present invention for the purpose of providing a multi-component separation pseudo moving bed type chromatographic separation method which is easy to control and inexpensive. .
【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、上記特許請求の範囲
の各請求項に記載した本発明方法を完成した。The present inventors have completed the method of the present invention as set forth in each claim of the above-mentioned claims in order to achieve the above objects.
【０００８】本発明方法の特徴は、代表的には、吸着剤
が充填された多数の充填塔を各々遮断弁を有する配管で
順次直列に連結した無端の充填塔群の系を、この吸着剤
に対して親和力が異なる３以上の成分を含む原料流体を
該系に流通させた時に形成される三つの区画（吸着剤に
対する親和力の強い成分（以下「成分Ｃ」という）の富
化された１乃至複数の充填塔群からなる第１区画、吸着
剤に対する親和力の中間の成分（以下「成分Ｂ」とい
う）の富化された１乃至複数の充填塔群及びこの吸着剤
に対する親和力の中間の成分Ｂと上記親和力の強い成分
Ｃが混合している１乃至複数の充填塔群からなる第２区
画、吸着剤に対する親和力の弱い成分（以下「成分Ａ」
という）が富化された１乃至複数の充填塔群を含む残り
の充填塔群からなる第３区画）に分けて、以下の，
，の工程を、，の順に交互に繰り返すか、ある
いは，，の順に繰り返すことにある。The feature of the method of the present invention is that, typically, a system of endless packed towers in which a large number of packed towers filled with adsorbents are sequentially connected in series by pipes each having a shutoff valve The three compartments (components having a strong affinity for the adsorbent (hereinafter referred to as “component C”) formed when a raw material fluid containing three or more components having different affinities to To a first section consisting of a plurality of packed tower groups, one or a plurality of packed tower groups enriched with a component having an intermediate affinity for the adsorbent (hereinafter referred to as “component B”), and a component having an intermediate affinity for the adsorbent A second section composed of one or a plurality of packed tower groups in which B and the above-mentioned component C having a strong affinity are mixed, a component having a weak affinity to the adsorbent (hereinafter referred to as "component A"
The third section consisting of the remaining packed tower group including one or a plurality of packed tower groups enriched with
The steps of and are alternately repeated in the order of, or they are repeated in the order of.
【０００９】 第２区画と第３区画の間の遮断弁を
閉じて系全体での流体の循環を遮断した状態で、この遮
断弁の直下流に位置する充填塔の入口から原料流体を供
給しながら第２区画内のいずれかの充填塔の出口から上
記成分Ｂの富化された画分を流出させる操作を行って、
第１区画〜第３区画の分布を少なくとも充填塔一つ分だ
け下流側に移行させる工程 上記の工程に続き、移行した第３区画と第１区
画の間の遮断弁を閉じた状態で、第１区画の最上流に位
置する充填塔の入口から脱着剤流体を供給しながら、該
第１区画の最下流の充填塔の出口から上記成分Ｃの富化
された画分を流出させる操作と、第３区画の最下流に位
置する充填塔の出口から上記成分Ａの富化された画分を
流出させる操作とを行い、更に第１区画〜第３区画の分
布が流体の下流側に１充填塔分だけ移行することに同期
して、脱着剤流体の供給位置、各画分の抜き出し位置、
及び遮断する遮断弁の位置を１充填塔分だけ繰り下げて
同じ操作を行うことを予め定めた回数繰り返す工程 上記の工程に続き、第３区画と第１区画の間の
遮断弁を閉じた状態で、第１区画の最上流に位置する充
填塔の入口から脱着剤流体を供給しながら、該第１区画
の最下流の充填塔の出口から上記成分Ｃの富化された画
分を流出させる操作と、第３区画の最下流に位置する充
填塔の出口から上記成分Ａの富化された画分を流出させ
る操作と、第２区画の最下流に位置する充填塔の出口か
ら上記成分Ｂの富化された画分を流出させる操作とを行
い、更に必要に応じて第１区画〜第３区画の分布が流体
の下流側に１充填塔分だけ移行することに同期して、脱
着剤流体の供給位置、各画分の抜き出し位置、及び遮断
する遮断弁の位置を１充填塔分だけ繰り下げて同じ操作
を行うことを予め定めた回数繰り返す工程。With the shutoff valve between the second and third compartments closed to shut off the circulation of the fluid in the entire system, the raw material fluid is supplied from the inlet of the packed column located immediately downstream of the shutoff valve. While performing the operation of flowing out the fraction enriched in the above component B from the outlet of any packed column in the second compartment,
Step of shifting the distribution of the first section to the third section to the downstream side by at least one packed column Continuing from the above step, with the shutoff valve between the transferred third section and the first section closed, An operation of supplying a desorbent fluid from an inlet of a packed column located at the uppermost stream of one section, and flowing out a fraction enriched in the component C from the outlet of the most downstream packed column of the first section; The operation of causing the fraction enriched in the component A to flow out from the outlet of the packed column located at the most downstream side of the third section, and further, the distribution of the first section to the third section is filled one downstream side of the fluid. In synchronism with the transfer of only the tower portion, the desorbent fluid supply position, each fraction extraction position,
And a step of repeating the same operation by lowering the position of the shutoff valve for shutting off by one packed tower and repeating the same operation a predetermined number of times. Following the above steps, with the shutoff valve between the third compartment and the first compartment closed. An operation of supplying the desorbent fluid from the inlet of the packed column located at the uppermost stream of the first section, while flowing out the fraction enriched in the component C from the outlet of the most downstream packed column of the first section. And an operation of flowing out the enriched fraction of the above component A from the outlet of the packed column located at the most downstream side of the third section, and the operation of the above component B from the outlet of the packed column located at the most downstream side of the second section. The operation of causing the enriched fraction to flow out is performed, and further, if necessary, the distribution of the first to third sections is synchronized with the transfer of one packed column to the downstream side of the fluid in synchronization with the desorbent fluid. The supply position of each, the extraction position of each fraction, and the position of the shut-off valve for shutting off each one packed column The step of repeating the same operation by moving back only a predetermined number of times.
【００１０】上記において、成分Ｃの富化された１乃至
複数の充填塔群からなる第１区画とは、該成分Ｃのみが
富化されたものであることを厳密に要求するものではな
い。例えば、主に分離回収しようとする成分がＢであっ
て、成分Ｃは除去のみを目的とすれば足りるような場合
には、この第１区画の最下流の充填塔内に成分Ｂが多少
混在していても差し支えないように、実施しようとする
目的、原料流体に含まれている成分の種類等に応じて第
１区画を形成する充填塔群を設定することができる。第
２区画、第３区画も同様である。In the above, the first section consisting of one or a plurality of packed tower groups enriched with the component C does not strictly require that only the component C is enriched. For example, when the component to be separated and recovered is B, and the component C only needs to be removed, the component B is somewhat mixed in the most downstream packed column of the first section. The packed tower group forming the first section can be set according to the purpose to be carried out, the type of components contained in the raw material fluid, etc. The same applies to the second section and the third section.
【００１１】上記のの工程においては、第１区画の最
上流の充填塔の入口から脱着剤流体を供給する操作、第
１区画の最下流の充填塔の出口から成分Ｃの富化された
画分を流出させる操作、第３区画の最下流の充填塔の出
口から成分Ａの富化された画分を流出させる操作、の少
なくともいずれかを同時又は順次に併せて行なってもよ
い。In the above process, the operation of supplying the desorbent fluid from the inlet of the most upstream packed column of the first section, the fraction enriched with the component C from the outlet of the most downstream packed column of the first section. At least one of the operation of flowing out the fraction and the operation of flowing out the fraction enriched in the component A from the outlet of the most downstream packed column in the third section may be performed simultaneously or sequentially in combination.
【００１２】また、上記の工程において閉じられる遮
断弁は、第２区画から第３区画への流体の流れを阻止で
きればこれらの区画の間の遮断弁に限定されるものでは
ない。したがってこの場合には、閉じた遮断弁の下流に
位置する第３区画内の比較的上流側に位置するいずれか
の充填塔の入口から原料流体を供給しながら、閉じた遮
断弁の上流に位置する第２区画内の比較的下流側に位置
するいずれかの充填塔の出口から上記成分Ｂの富化され
た画分を流出させることができる。ここで原料流体を供
給する充填塔が第３区画の比較的上流のものであるとい
うのは、成分Ａの分布状態やその性質によって第３区画
の最上流の充填塔でなくともよいという意味であり、一
般的には最上流の充填塔か、その次ぎの下流の充填塔が
選ばれるが、充填塔の設置本数等によってはこれに限定
されるものではない。同様に、上記成分Ｂを流出させる
充填塔が、第２区画内の比較的下流側に位置するという
のは、一般的には第２区画内の最下流の充填塔か、その
すぐ上流の充填塔が選ばれるが、充填塔の設置本数等に
よってはこれに限定されるものではない。The shutoff valve closed in the above step is not limited to the shutoff valve between these compartments as long as it can block the flow of fluid from the second compartment to the third compartment. Therefore, in this case, while the raw material fluid is supplied from the inlet of one of the packed towers located relatively upstream in the third section located downstream of the closed shutoff valve, the raw material fluid is supplied upstream of the closed shutoff valve. The fraction enriched in the component B can be discharged from the outlet of any one of the packed columns located relatively downstream in the second section. Here, the fact that the packed tower for supplying the raw material fluid is relatively upstream of the third section means that the packed tower does not have to be the uppermost packed tower in the third section, depending on the distribution state of component A and its nature. In general, the most upstream packed tower or the next packed tower downstream thereof is selected, but it is not limited to this depending on the number of installed packed towers and the like. Similarly, the packed column for discharging the component B is located relatively downstream in the second section, generally because the packed column located at the most downstream side in the second section or immediately upstream of the packed tower. A tower is selected, but it is not limited to this depending on the number of installed packed towers and the like.
【００１３】また、上記のの工程においては、この工
程の前及び又は後に、第１区画の最上流に位置する充填
塔の入口から脱着剤流体を供給しながら、該第１区画の
最下流の充填塔の出口から上記成分Ｃの富化された画分
を流出させる操作と、第１区画の最上流に位置する充填
塔の入口から脱着剤流体を供給しながら、第３区画の最
下流に位置する充填塔の出口から上記成分Ａの富化され
た画分を流出させる操作とを、同時に行なうか、順次に
行なうか、あるいはこれらの操作を同時に行うことに加
えて更にこれらの操作の少なくともいずれかを順次に行
なうようにしてもよい。In the above step, before and / or after this step, while supplying the desorbent fluid from the inlet of the packed column located at the uppermost stream of the first section, the most downstream of the first section is supplied. The operation of letting out the fraction enriched in the above component C from the outlet of the packed column, and supplying the desorbent fluid from the inlet of the packed column located at the uppermost stream of the first section, to the most downstream of the third section. The operation of flowing out the fraction enriched in the component A from the outlet of the packed column located at the same time, sequentially, or simultaneously performing these operations, and at least these operations Either may be performed sequentially.
【００１４】また更に、繰り返して行なわれるの工程
において、あるいは該の工程とこれに続いて行なわれ
るの工程において、各繰り返し毎の操作に先立ち、系
内の遮断弁をいずれも開とした状態で、第１区画の最上
流に位置する充填塔の入口から脱着剤流体を供給しなが
ら、第１区画の最下流に位置する充填塔の出口から成分
Ｃの富化された画分を流出させる操作を行なうようにす
ることも好ましい。In addition, in the repeated steps, or in the step and the subsequent steps, the shut-off valves in the system are all opened before the operation of each repetition. An operation of supplying the desorbent fluid from the inlet of the packed column located at the uppermost stream of the first section, while flowing out the fraction enriched in the component C from the outlet of the packed column located at the most downstream side of the first section. It is also preferable to perform.
【００１５】[0015]
【発明の効果】本発明の方法によれば、充填塔群の系を
４つの区画に分けていた従来法に比べ、その区画数が１
少ない３となるために、吸着剤に対する親和力が弱い成
分の画分を流出させるための流量制御が不要になるとい
う効果がある。According to the method of the present invention, the number of sections is 1 as compared with the conventional method in which the system of the packed tower group is divided into 4 sections.
Since the number is 3 which is small, there is an effect that the flow rate control for flowing out the fraction of the component having a weak affinity for the adsorbent becomes unnecessary.
【００１６】また、第３区画と第１区画の遮断弁を閉じ
ず、第３区画の最後列に位置する充填塔からの流体を第
１区画の最前列に位置する充填塔に供給する工程をつけ
加えたことにより、脱着剤の使用量を減らすことができ
るという効果がある。Further, a step of supplying the fluid from the packed column located in the last row of the third section to the packed column located in the front row of the first section without closing the shutoff valves of the third section and the first section With the addition, there is an effect that the amount of the desorbent used can be reduced.
【００１７】さらにまた、吸着剤に対する親和力が強い
成分のみを流出させる工程、及び／又は吸着剤に対する
親和力が弱い成分のみを流出させる工程をつけ加えた方
法においては、分離性能を向上させることができるとい
う効果がある。Furthermore, it is said that the separation performance can be improved by adding a step of flowing out only a component having a strong affinity to the adsorbent and / or a step of flowing out only a component having a weak affinity to the adsorbent. effective.
【００１８】[0018]
【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。EXAMPLES The present invention will be described in detail below based on examples, but it goes without saying that the present invention is not limited to these examples.
【００１９】実施例１ （マルトトリオースとマルトー
スとグルコースの分離） 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。Example 1 (maltotriose and malteau)
Separation of glucose and glucose) FIG. 1 is an explanatory view showing the flow of the apparatus used in this example.
【００２０】内径３．７ｃｍ、長さ５０ｃｍの充填塔Ｔ
（Ｔ１．．．．Ｔ８）８本のそれぞれの末端を次の充填
塔の頂部に遮断弁Ｋ（Ｋ１．．．．Ｋ８）を介して配管
Ｈで無端連結し、各遮断弁Ｋの上流側の配管ＨにＡ液流
出弁Ａ（Ａ１．．．．Ａ８）とＢ液流出弁Ｂ（Ｂ４，Ｂ
５，Ｂ６）とＣ液流出弁Ｃ（Ｃ１．．．．Ｃ８）と循環
弁Ｍ（Ｍ１．．．．Ｍ８）を連結するとともに、各遮断
弁Ｋの下流側の配管Ｈに原液供給弁Ｆ（Ｆ１．．．．Ｆ
８）と溶離液供給弁Ｄ（Ｄ１．．．．Ｄ８）を連結し、
さらに循環弁Ｍの他端を溶離液ポンプＰ１１の入口に連
結し、かつ該連結部の上流側に逆止弁を設置した実験装
置を用いた。なお、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型を充填した。A packed tower T having an inner diameter of 3.7 cm and a length of 50 cm
(T1 ... T8) Each of the eight ends is connected endlessly to the top of the next packed column via a shutoff valve K (K1 ... K8) with a pipe H, upstream of each shutoff valve K. The liquid A outflow valve A (A1 ... A8) and the liquid B outflow valve B (B4, B
5, B6), the C liquid outflow valve C (C1 ... C8) and the circulation valve M (M1 ... M8) are connected, and the stock solution supply valve F is connected to the pipe H on the downstream side of each shutoff valve K. (F1 ... F
8) and the eluent supply valve D (D1 ... D8) are connected,
Furthermore, an experimental apparatus was used in which the other end of the circulation valve M was connected to the inlet of the eluent pump P11, and a check valve was installed on the upstream side of the connecting portion. Each packed column was filled with the strongly acidic cation exchange resin Amberlite CG-6000 Na type.
【００２１】なお、遮断弁は常時開、各供給弁、各流出
弁、循環弁は常時閉の弁であり特に記述しない限りは常
時の状態とした。The shutoff valve is a normally open valve, each supply valve, each outflow valve, and the circulation valve are normally closed valves.
【００２２】１工程として、遮断弁Ｋ５を作動させて充
填塔５と６の間の流れを遮断し、原液供給弁Ｆ６を開い
て充填塔Ｔ６の頂部から原液を導入し、溶離液供給弁Ｄ
１を開いて充填塔Ｔ１の頂部から溶離液として水を導入
し、Ｂ液流出弁Ｂ５を開き充填塔Ｔ５の底部からマルト
ースを多く含む液（Ｂ液）を抜き出した。As one step, the shutoff valve K5 is operated to shut off the flow between the packed towers 5 and 6, the stock solution supply valve F6 is opened to introduce the stock solution from the top of the packed tower T6, and the eluent supply valve D
1 was opened to introduce water as an eluent from the top of the packed tower T1, and the B solution outflow valve B5 was opened to withdraw a solution containing a large amount of maltose (B solution) from the bottom of the packed tower T5.
【００２３】あらかじめ定めた時間を経過した後、２工
程として、遮断弁Ｋ１を閉とし、溶離液供給弁Ｄ２、Ａ
液流出弁Ａ１、Ｃ液流出弁Ｃ３を開とした。After a lapse of a predetermined time, the shutoff valve K1 is closed and the eluent supply valves D2 and A2 are closed in two steps.
The liquid outflow valves A1 and C were opened.
【００２４】以下、８工程まで、遮断する遮断弁および
開とする溶離液供給弁、Ａ液流出弁、Ｃ液流出弁を順次
液の流れ方向に沿って移動させた。なお、本実施例１で
は循環弁Ｍは全工程で閉とした。In the following, until the 8th step, the shut-off valve for shutting off, the eluent supply valve for opening, the A liquid outflow valve, and the C liquid outflow valve were sequentially moved in the liquid flow direction. In the first embodiment, the circulation valve M is closed in all steps.
【００２５】上記の１工程から８工程までを１サイクル
として２１サイクル繰り返した。21 cycles were repeated with the above steps 1 to 8 as one cycle.
【００２６】原液組成、運転条件を下記表１に、また回
収された各画分の組成を下記表２に示した。The stock solution composition and operating conditions are shown in Table 1 below, and the composition of each recovered fraction is shown in Table 2 below.
【００２７】[0027]
【表１】 [Table 1]
【００２８】[0028]
【表２】 [Table 2]
【００２９】実施例２ 本実施例においても第１図の装置を使用した。Example 2 The apparatus of FIG. 1 was used also in this example.
【００３０】なお、遮断弁は常時開、各供給弁、各流出
弁、循環弁は常時閉の弁であり特に記述しない限りは常
時の状態とした。The shut-off valve is normally open, and each supply valve, each outflow valve, and the circulation valve are normally closed.
【００３１】１工程として、遮断弁Ｋ５を作動させて充
填塔５と６の間の流れを遮断し、原液供給弁Ｆ６を開い
て充填塔Ｔ６の頂部から原液を導入し、Ｂ液流出弁Ｂ５
を開き充填塔Ｔ５の底部からマルトースを多く含む液
（Ｂ液）を抜き出した。As one step, the shutoff valve K5 is operated to shut off the flow between the packed towers 5 and 6, the stock solution supply valve F6 is opened to introduce the stock solution from the top of the packed tower T6, and the solution B outflow valve B5.
The liquid containing a large amount of maltose (liquid B) was extracted from the bottom of the packed tower T5.
【００３２】あらかじめ定めた時間を経過した後、２工
程の１として、遮断弁Ｋ１を閉とし、循環弁Ｍ１、溶離
液供給弁Ｄ２、Ｃ液流出弁Ｃ３を開とした。一定時間経
過後、２工程の２として、２工程の１に追加して、循環
弁Ｍ１を閉とし、Ａ液流出弁Ａ１を開とした。After the elapse of a predetermined time, the shutoff valve K1 was closed and the circulation valve M1, the eluent supply valve D2, and the C liquid outflow valve C3 were opened as 1 of 2 steps. After the lapse of a certain period of time, as 2 of 2 steps, in addition to 1 of 2 steps, the circulation valve M1 was closed and the A liquid outflow valve A1 was opened.
【００３３】以下同様に、８工程まで、遮断する遮断
弁、開閉する循環弁、および開とする溶離液供給弁、Ａ
液流出弁、Ｃ液流出弁を順次液の流れ方向に沿って移動
させた。Similarly, up to 8 steps, a shutoff valve that shuts off, a circulation valve that opens and closes, and an eluent supply valve that opens, A
The liquid outflow valve and the C liquid outflow valve were sequentially moved along the liquid flow direction.
【００３４】上記の１工程から８工程までを１サイクル
として２１サイクル繰り返した。The above steps 1 to 8 were set as one cycle, and 21 cycles were repeated.
【００３５】原液組成、運転条件を下記表３に、また回
収された各画分の組成を下記表４に示した。The stock solution composition and operating conditions are shown in Table 3 below, and the composition of each recovered fraction is shown in Table 4 below.
【００３６】[0036]
【表３】 [Table 3]
【００３７】[0037]
【表４】 [Table 4]
【００３８】弁の開閉の一巡すなわち１工程から８工程
までを１サイクルとしたとき、２１サイクル後の流出液
の組成は表４の通りであり、実施例１に較べて、溶離液
の使用量が減少した分Ａ画分の濃度が上昇した。The composition of the effluent after 21 cycles is as shown in Table 4 when one cycle of opening and closing of the valve, that is, from 1 step to 8 steps is defined as Table 4, and the amount of the eluent used is larger than that in Example 1. The concentration of the fraction A was increased.
【００３９】実施例３ 本実施例においても第１図の装置を使用した。Example 3 The apparatus of FIG. 1 was used also in this example.
【００４０】なお、遮断弁は常時開、各供給弁、各流出
弁、循環弁は常時閉の弁であり特に記述しない限りは常
時の状態とした。The shut-off valve is normally open, each supply valve, each outflow valve, and the circulation valve are normally closed. Unless otherwise specified, they are in the normal state.
【００４１】１工程として、遮断弁Ｋ５を作動させて充
填塔５と６の間の流れを遮断し、原液供給弁Ｆ６を開い
て充填塔Ｔ６の頂部から原液を導入し、Ｂ液流出弁Ｂ５
を開き充填塔Ｔ５の底部からマルトースを多く含む液
（Ｂ液）を抜き出した。As one step, the shutoff valve K5 is operated to shut off the flow between the packed towers 5 and 6, the stock solution supply valve F6 is opened to introduce the stock solution from the top of the packed tower T6, and the solution B outflow valve B5.
The liquid containing a large amount of maltose (liquid B) was extracted from the bottom of the packed tower T5.
【００４２】あらかじめ定めた時間を経過した後、２工
程の１として、遮断弁Ｋ１を閉とし、循環弁Ｍ１、溶離
液供給弁Ｄ２、Ｃ液流出弁Ｃ３を開とした（第３区画か
らの流出液を第１区画に供給）。After the elapse of a predetermined time, the shutoff valve K1 is closed and the circulation valve M1, the eluent supply valve D2, and the C liquid outflow valve C3 are opened as one of the two steps (from the third section). Supply effluent to the first compartment).
【００４３】一定時間経過後、２工程の２として、２工
程の１に追加して、遮断弁Ｋ１、循環弁Ｍ１を閉とした
（Ｃのみ抜き出し）。After the elapse of a certain time, as 2 of 2 steps, in addition to 1 of 2 steps, the shutoff valve K1 and the circulation valve M1 were closed (only C was extracted).
【００４４】一定時間経過後、２工程の３として、２工
程の２に追加して、Ａ液流出弁Ａ１を開とした（ＡとＣ
の抜き出し）。After the elapse of a certain time, in addition to step 2 of step 2 as step 3, the liquid A outflow valve A1 was opened (A and C).
Extraction).
【００４５】一定時間経過後、２工程の４として、２工
程の３で開となっていたＣ液流出弁Ｃ３を閉とし、他の
弁はそのままとした（Ａのみ抜き出し）。After the elapse of a certain time, the liquid C outflow valve C3, which was opened in 3 of 2 process, was closed in 4 of 2 process, and the other valves were left as they were (only A was extracted).
【００４６】以下、８工程まで、開閉する遮断弁、循環
弁、溶離液供給弁、Ａ液流出弁、Ｃ液流出弁を順次液の
流れ方向に沿って移動させた。In the following, up to 8 steps, the shutoff valve, the circulation valve, the eluent supply valve, the A liquid outflow valve, and the C liquid outflow valve which were opened and closed were sequentially moved in the liquid flow direction.
【００４７】上記の１工程から８工程までを１サイクル
として２０サイクル繰り返した。The above steps 1 to 8 were set as one cycle, and 20 cycles were repeated.
【００４８】原液組成、運転条件を下記表５に、また回
収された各画分の組成を下記表６に示した。The stock solution composition and operating conditions are shown in Table 5 below, and the composition of each recovered fraction is shown in Table 6 below.
【００４９】[0049]
【表５】 [Table 5]
【００５０】[0050]
【表６】 [Table 6]
【００５１】弁の開閉の一巡すなわち１工程から８工程
までを１サイクルとしたとき、２０サイクル後の流出液
の組成は表６の通りであり、実施例１および実施例２に
較べ各区画の目的成分の純度が向上した。The composition of the effluent after 20 cycles is as shown in Table 6 when one cycle of opening and closing the valve, that is, 1st to 8th steps is defined as one cycle. The purity of the target component is improved.
【図１】第１図は実施例に用いた装置の構成概要示した
説明図である。FIG. 1 is an explanatory diagram showing a schematic configuration of a device used in an embodiment.
【図２】第２図は実施例１の操作フロー及び各成分の分
布を示した説明図である。FIG. 2 is an explanatory diagram showing an operation flow and a distribution of each component of the first embodiment.
【図３】第３図（ａ）は実施例２の操作フロー及び各成
分の分布を示した説明図である。FIG. 3 (a) is an explanatory diagram showing the operation flow and the distribution of each component of Example 2.
【図４】第３図（ｂ）は実施例２の操作フロー及び各成
分の分布を示した説明図である。FIG. 3 (b) is an explanatory view showing the operation flow and the distribution of each component of the second embodiment.
【図５】第４図（ａ）は実施例３の操作フロー及び各成
分の分布を示した説明図である。FIG. 5 (a) is an explanatory diagram showing an operation flow of Example 3 and distributions of respective components.
【図６】第４図（ｂ）は実施例３の操作フロー及び各成
分の分布を示した説明図である。FIG. 4 (b) is an explanatory view showing the operation flow and the distribution of each component of Example 3.
【図７】第４図（ｃ）は実施例３の操作フロー及び各成
分の分布を示した説明図である。FIG. 7 (c) is an explanatory diagram showing the operation flow and the distribution of each component of Example 3.
【図８】第４図（ｄ）は実施例３の操作フロー及び各成
分の分布を示した説明図である。FIG. 4 (d) is an explanatory diagram showing the operation flow and the distribution of each component of Example 3.
Ｔ１〜Ｔ８：充填塔、Ａ１〜Ａ８：Ａ液流出弁、Ａ９：
背圧弁 Ｂ４〜Ｂ６：Ｂ液流出弁、Ｃ１〜Ｃ８：Ｃ液流出弁、Ｄ
１〜Ｄ８：溶離液供給弁、Ｄ９：逆止弁、Ｆ１〜Ｆ８：
原液供給弁 Ｋ１〜Ｋ８：遮断弁、Ｍ１〜Ｍ８：循環弁、Ｐ１１：溶
離液供給ポンプ Ｐ１２：原液供給ポンプ、 Ｐ１３：Ｃ液抜き出しポン
プ、Ｈ：充填塔接続配管、Ｉ：Ｂ液抜き出し配管、Ｊ：
循環配管。T1 to T8: packed tower, A1 to A8: A liquid outflow valve, A9:
Back pressure valve B4 to B6: B liquid outflow valve, C1 to C8: C liquid outflow valve, D
1 to D8: eluent supply valve, D9: check valve, F1 to F8:
Stock solution supply valve K1 to K8: Shutoff valve, M1 to M8: Circulation valve, P11: Eluent solution supply pump P12: Stock solution supply pump, P13: C solution extraction pump, H: Packing tower connection pipe, I: B solution extraction pipe, J:
Circulation piping.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成５年１０月４日[Submission date] October 4, 1993
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】図面[Document name to be corrected] Drawing
【補正対象項目名】図３[Name of item to be corrected] Figure 3
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図３】 [Figure 3]
【手続補正２】[Procedure Amendment 2]
【補正対象書類名】図面[Document name to be corrected] Drawing
【補正対象項目名】図４[Name of item to be corrected] Fig. 4
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図４】 [Figure 4]
【手続補正３】[Procedure 3]
【補正対象書類名】図面[Document name to be corrected] Drawing
【補正対象項目名】図５[Name of item to be corrected] Figure 5
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図５】 [Figure 5]
【手続補正４】[Procedure amendment 4]
【補正対象書類名】図面[Document name to be corrected] Drawing
【補正対象項目名】図６[Name of item to be corrected] Figure 6
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図６】 [Figure 6]
【手続補正５】[Procedure Amendment 5]
【補正対象書類名】図面[Document name to be corrected] Drawing
【補正対象項目名】図７[Name of item to be corrected] Figure 7
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図７】 [Figure 7]
【手続補正６】[Procedure correction 6]
【補正対象書類名】図面[Document name to be corrected] Drawing
【補正対象項目名】図８[Correction target item name] Figure 8
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図８】 [Figure 8]
【手続補正７】[Procedure Amendment 7]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】図面の簡単な説明[Name of item to be corrected] Brief description of the drawing
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図面の簡単な説明】[Brief description of drawings]
【図１】第１図は実施例に用いた装置の構成概要示した
説明図である。FIG. 1 is an explanatory diagram showing a schematic configuration of a device used in an embodiment.
【図２】第２図は実施例１の操作フロー及び各成分の分
布を示した説明図である。FIG. 2 is an explanatory diagram showing an operation flow and a distribution of each component of the first embodiment.
【図３】第３図は実施例２の操作フロー及び各成分の分
布を示した説明図である。FIG. 3 is an explanatory diagram showing an operation flow and a distribution of each component of the second embodiment.
【図４】第４図は実施例２の操作フロー及び各成分の分
布を示した説明図である。[4] FIG. 4 is an explanatory view showing the distribution of the operation flows and the ingredients of Example 2.
【図５】第５図は実施例３の操作フロー及び各成分の分
布を示した説明図である。[5] FIG. 5 is an explanatory view showing the distribution of the operation flows and the ingredients of Example 3.
【図６】第６図は実施例３の操作フロー及び各成分の分
布を示した説明図である。[6] FIG. 6 is an explanatory diagram showing the distribution of the operation flows and the ingredients of Example 3.
【図７】第７図は実施例３の操作フロー及び各成分の分
布を示した説明図である。[Figure 7] Figure 7 is an explanatory view showing the distribution of the operation flows and the ingredients of Example 3.
【図８】第８図は実施例３の操作フロー及び各成分の分
布を示した説明図である。[Figure 8] Figure 8 is an explanatory view showing the distribution of the operation flows and the ingredients of Example 3.
【符号の説明】 Ｔ１〜Ｔ８：充填塔、Ａ１〜Ａ８：Ａ液流出弁、Ａ９：
背圧弁 Ｂ４〜Ｂ６：Ｂ液流出弁、Ｃ１〜Ｃ８：Ｃ液流出弁、Ｄ
１〜Ｄ８：溶離液供給弁、Ｄ９：逆止弁、Ｆ１〜Ｆ８：
原液供給弁 Ｋ１〜Ｋ８：遮断弁、Ｍ１〜Ｍ８：循環弁、Ｐ１１：溶
離液供給ポンプ Ｐ１２：原液供給ポンプ、 Ｐ１３：Ｃ液抜き出しポン
プ、Ｈ：充填塔接続配管、Ｉ：Ｂ液抜き出し配管、Ｊ：
循環配管。[Explanation of Codes] T1 to T8: Packing tower, A1 to A8: A liquid outflow valve, A9:
Back pressure valve B4 to B6: B liquid outflow valve, C1 to C8: C liquid outflow valve, D
1 to D8: eluent supply valve, D9: check valve, F1 to F8:
Stock solution supply valve K1 to K8: Shutoff valve, M1 to M8: Circulation valve, P11: Eluent solution supply pump P12: Stock solution supply pump, P13: C solution extraction pump, H: Packing tower connection pipe, I: B solution extraction pipe, J:
Circulation piping.
フロントページの続き (72)発明者 金子 菊造 東京都文京区本郷５丁目５番16号 オルガ ノ株式会社内Front page continuation (72) Inventor Kikuzo Kaneko 5-5-16 Hongo, Bunkyo-ku, Tokyo Organo Corporation
Claims (5)
遮断弁を有する配管で順次直列に連結した無端の充填塔
群の系を、この吸着剤に対して親和力が異なる３以上の
成分を含む原料流体を該系に流通させた時に形成される
三つの区画（吸着剤に対する親和力の強い成分の富化さ
れた１乃至複数の充填塔群からなる第１区画、吸着剤に
対する親和力の中間の成分の富化された１乃至複数の充
填塔群及びこの吸着剤に対する親和力の中間の成分と上
記親和力の強い成分が混合している１乃至複数の充填塔
群からなる第２区画、吸着剤に対する親和力の弱い成分
が富化された１乃至複数の充填塔群を含む残りの充填塔
群からなる第３区画）に分けて、以下の，，の工
程を、，の順に交互に繰り返すか、あるいは，
，の順に繰り返すことを特徴とするクロマト分離法 第２区画と第３区画の間の遮断弁を閉じて系全体
での流体の循環を遮断した状態で、この遮断弁の直下流
に位置する充填塔の入口から原料流体を供給しながら第
２区画内のいずれかの充填塔の出口から上記親和力の中
間の成分の富化された画分を流出させる操作を行って、
第１区画〜第３区画の分布を少なくとも充填塔一つ分だ
け下流側に移行させる工程 上記の工程に続き、移行した第３区画と第１区
画の間の遮断弁を閉じた状態で、第１区画の最上流に位
置する充填塔の入口から脱着剤流体を供給しながら、該
第１区画の最下流の充填塔の出口から上記親和力の強い
成分の富化された画分を流出させる操作と、第３区画の
最下流に位置する充填塔の出口から上記親和力の弱い成
分の富化された画分を流出させる操作とを行い、更に第
１区画〜第３区画の分布が流体の下流側に１充填塔分だ
け移行することに同期して、脱着剤流体の供給位置、各
画分の抜き出し位置、及び遮断する遮断弁の位置を１充
填塔分だけ繰り下げて同じ操作を行うことを予め定めた
回数繰り返す工程 上記の工程に続き、第３区画と第１区画の間の
遮断弁を閉じた状態で、第１区画の最上流に位置する充
填塔の入口から脱着剤流体を供給しながら、該第１区画
の最下流の充填塔の出口から上記親和力の強い成分の富
化された画分を流出させる操作と、第３区画の最下流に
位置する充填塔の出口から上記親和力の弱い成分の富化
された画分を流出させる操作と、第２区画の最下流に位
置する充填塔の出口から上記親和力の中間の成分の富化
された画分を流出させる操作とを行い、更に必要に応じ
て第１区画〜第３区画の分布が流体の下流側に１充填塔
分だけ移行することに同期して、脱着剤流体の供給位
置、各画分の抜き出し位置、及び遮断する遮断弁の位置
を１充填塔分だけ繰り下げて同じ操作を行うことを予め
定めた回数繰り返す工程。1. A system of endless packed towers in which a large number of packed towers filled with an adsorbent are sequentially connected in series by pipes each having a shutoff valve, and three or more components having different affinities for the adsorbent are provided. Three compartments formed when a raw material fluid containing a is passed through the system (first compartment consisting of one or a plurality of packed tower groups enriched with components having a strong affinity for the adsorbent, intermediate affinity for the adsorbent) Adsorbent, which is composed of one or a plurality of packed tower groups enriched with the above components, and one or a plurality of packed tower groups in which a component having an intermediate affinity for this adsorbent and a component having a strong affinity are mixed. The third step consisting of the remaining packed tower group including one or a plurality of packed tower groups enriched with a component having a weak affinity for Alternatively,
The chromatographic separation method is characterized by repeating in the order of, and the packing located immediately downstream of the shut-off valve with the shut-off valve between the second and third compartments closed to shut off the fluid circulation in the entire system. Performing an operation of flowing out a fraction enriched in the intermediate component of the affinity from the outlet of any packed column in the second compartment while supplying the raw material fluid from the inlet of the column,
Step of shifting the distribution of the first section to the third section to the downstream side by at least one packed column Continuing from the above step, with the shutoff valve between the transferred third section and the first section closed, An operation of supplying a desorbent fluid from an inlet of a packed column located at the uppermost stream of one section, and flowing out a fraction enriched with the component having high affinity from the outlet of the most downstream packed column of the first section. And the operation of flowing out the fraction enriched with the component having a weak affinity from the outlet of the packed column located at the most downstream side of the third section, and the distribution of the first section to the third section is further downstream of the fluid. In synchronism with the transfer of only one packed column to the side, the same operation is performed by lowering the supply position of the desorbent fluid, the extraction position of each fraction, and the position of the shutoff valve for shutting off by one packed column. Steps repeated a predetermined number of times Following the above steps, the third section and the first section While the shutoff valve between the compartments is closed, the desorbent fluid is supplied from the inlet of the packed column located in the uppermost stream of the first section, and the affinity of the affinity is increased from the outlet of the most packed column in the first section. An operation of flowing out a fraction enriched in a strong component, an operation of flowing out a fraction enriched in a component having a weak affinity described above from an outlet of a packed column located at the most downstream side of the third compartment, and a second compartment The operation of flowing out the enriched fraction of the component having the intermediate affinity is performed from the outlet of the packed column located at the most downstream side of the column, and if necessary, the distribution of the first section to the third section is downstream of the fluid. In synchronism with the transfer of only one packed column to the side, the same operation is performed by lowering the supply position of the desorbent fluid, the extraction position of each fraction, and the position of the shutoff valve for shutting off by one packed column. A process of repeating a predetermined number of times.
の最上流の充填塔の入口から脱着剤流体を供給する操
作、第１区画の最下流の充填塔の出口から吸着剤に対す
る親和力の強い成分の富化された画分を流出させる操
作、第３区画の最下流の充填塔の出口から吸着剤に対す
る親和力の弱い成分の富化された画分を流出させる操
作、の少なくともいずれかを同時又は順次に併せて行な
うことを特徴とするクロマト分離法。2. The process according to claim 1, wherein the desorbent fluid is supplied from the inlet of the most upstream packed column in the first section, and the affinity for the adsorbent is adjusted from the outlet of the most downstream packed column in the first section. At least one of an operation of flowing out a fraction enriched in a strong component and an operation of flowing out a fraction enriched in a component having a weak affinity for an adsorbent from the outlet of the packed column at the most downstream side of the third section. A chromatographic separation method characterized by being performed simultaneously or sequentially.
えて、第２区画から第３区画への流体の流れを阻止する
ように上記系内の遮断弁のいずれかを閉じた状態で、こ
の遮断弁の下流に位置する第３区画内の上流側に位置す
るいずれかの充填塔の入口から原料流体を供給しなが
ら、遮断弁の上流に位置する第２区画内の下流側に位置
するいずれかの充填塔の出口から上記中間の成分の富化
された画分を流出させる操作を行って、第１区画〜第３
区画の分布を少なくとも充填塔一つ分だけ下流側に移行
させる´の工程を有することを特徴とするクロマト分
離法。3. The process according to claim 1 or 2, in which the shutoff valve in the system is closed so as to prevent the flow of fluid from the second compartment to the third compartment, instead of the step of While being supplied with the raw material fluid from the inlet of one of the packed towers located on the upstream side in the third compartment located downstream of this shutoff valve, it is located on the downstream side in the second compartment located upstream of the shutoff valve The first compartment to the third compartment is operated by flowing out the fraction enriched in the intermediate component from the outlet of any of the packed towers.
A chromatographic separation method comprising the step of shifting the distribution of compartments to the downstream side by at least one packed column.
の前及び又は後に、第３区画と第１区画の間の遮断弁を
閉じた状態で、第１区画の最上流に位置する充填塔の入
口から脱着剤流体を供給しながら、該第１区画の最下流
の充填塔の出口から上記親和力の強い成分の富化された
画分を流出させる操作と、第１区画の最上流に位置する
充填塔の入口から脱着剤流体を供給しながら、第３区画
の最下流に位置する充填塔の出口から上記親和力の弱い
成分の富化された画分を流出させる操作とを、同時に行
なうか、順次に行なうか、あるいはこれらの操作を同時
に行うことに加えて更にこれらの操作の少なくともいず
れかを順次に行なうことを特徴とするクロマト分離法。4. A filling located upstream of the first compartment with the shutoff valve between the third compartment and the first compartment closed before and / or after the step of any one of claims 1 to 3. An operation of causing the enriched fraction of the component having a strong affinity to flow out from the outlet of the packed column at the most downstream side of the first compartment while supplying the desorbent fluid from the inlet of the tower; While supplying the desorbent fluid from the inlet of the packed tower located at the same time, the operation of causing the enriched fraction of the component having a weak affinity to flow out from the outlet of the packed tower located at the most downstream side of the third section is simultaneously performed. A chromatographic separation method, characterized in that it is performed sequentially, or at least one of these operations is performed in addition to performing these operations simultaneously.
繰り返して行なわれるの工程、あるいは該の工程及
びこれに続いて行なわれるの工程、の各繰り返し毎の
操作に先立ち、系内の遮断弁をいずれも開とした状態
で、第１区画の最上流に位置する充填塔の入口から脱着
剤流体を供給しながら、第１区画の最下流に位置する充
填塔の出口から吸着剤に対する親和力が強い成分の富化
された画分を流出させる操作を行なうことを特徴とする
クロマト分離法。5. The method according to any one of claims 1 to 4,
Prior to the operation of each of the repeated steps, or the step and the subsequent steps, with the shut-off valves in the system open, the uppermost stream of the first compartment While supplying the desorbent fluid from the inlet of the packed tower located at 1, the fraction enriched with the component having a strong affinity for the adsorbent is discharged from the outlet of the packed tower located at the most downstream side of the first section. A chromatographic separation method characterized by the above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32311691A JP2968107B2 (en) | 1991-12-06 | 1991-12-06 | Chromatographic separation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32311691A JP2968107B2 (en) | 1991-12-06 | 1991-12-06 | Chromatographic separation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0716401A true JPH0716401A (en) | 1995-01-20 |
| JP2968107B2 JP2968107B2 (en) | 1999-10-25 |
Family
ID=18151265
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32311691A Expired - Lifetime JP2968107B2 (en) | 1991-12-06 | 1991-12-06 | Chromatographic separation method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2968107B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001334103A (en) * | 2000-05-26 | 2001-12-04 | Japan Organo Co Ltd | Chromatograph type separation device |
| US6437654B2 (en) | 1997-11-19 | 2002-08-20 | Nec Corporation | Substrate-type non-reciprocal circuit element and integrated circuit having multiple ground surface electrodes and co-planar electrical interface |
| JP2013523107A (en) * | 2010-03-30 | 2013-06-17 | デュポン ニュートリション バイオサイエンシーズ エーピーエス | Separation method |
-
1991
- 1991-12-06 JP JP32311691A patent/JP2968107B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6437654B2 (en) | 1997-11-19 | 2002-08-20 | Nec Corporation | Substrate-type non-reciprocal circuit element and integrated circuit having multiple ground surface electrodes and co-planar electrical interface |
| JP2001334103A (en) * | 2000-05-26 | 2001-12-04 | Japan Organo Co Ltd | Chromatograph type separation device |
| JP4632327B2 (en) * | 2000-05-26 | 2011-02-16 | オルガノ株式会社 | Chromatographic separation device |
| JP2013523107A (en) * | 2010-03-30 | 2013-06-17 | デュポン ニュートリション バイオサイエンシーズ エーピーエス | Separation method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2968107B2 (en) | 1999-10-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5198120A (en) | Process for fractional separation of multi-component fluid mixture | |
| FI81268B (en) | KONTINUERLIGT SEPARATIONSFOERFARANDE BASERAT PAO SERIESTROEMNING. | |
| JP4627841B2 (en) | Psicose separation method | |
| JP2962594B2 (en) | How to separate multiple components | |
| WO2005097286A1 (en) | Chromatographic separation equipment | |
| JP4945364B2 (en) | Separation method of sugar alcohol | |
| JPH0716401A (en) | Chromatographic separation | |
| JP2017205721A (en) | Chromatographic separation method and device for separating multicomponent into three or more fraction | |
| JP3277575B2 (en) | Chromatographic separation method | |
| JP2740780B2 (en) | Simulated moving bed equipment | |
| JPS60500203A (en) | How to prevent adsorption bed compaction | |
| JP4606092B2 (en) | Pseudo moving bed type chromatographic separation method and apparatus | |
| JP3359762B2 (en) | How to separate multiple components | |
| JP4603114B2 (en) | Method and apparatus for separating a plurality of components contained in a liquid | |
| JP4632327B2 (en) | Chromatographic separation device | |
| JPH0724724B2 (en) | Method and apparatus for separating multi-component system | |
| JP2965747B2 (en) | Multicomponent separation method and apparatus | |
| JP2012098052A (en) | Method and apparatus for chromatographic separation | |
| JP2834225B2 (en) | Simulated moving bed chromatographic separator | |
| JP3256349B2 (en) | Separation method and apparatus using simulated moving bed | |
| JP3256390B2 (en) | How to separate multiple components | |
| JP2879961B2 (en) | Chromatographic separation method and simplified simulated moving bed apparatus | |
| JP2962593B2 (en) | How to separate multiple components | |
| JP4395222B2 (en) | Method and apparatus for separating a plurality of components contained in a liquid | |
| JPH03100459A (en) | Pseudo moving bed type chromato separation |
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 (prs date is renewal date of database) |
Year of fee payment: 9 Free format text: PAYMENT UNTIL: 20080820 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 9 Free format text: PAYMENT UNTIL: 20080820 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 10 Free format text: PAYMENT UNTIL: 20090820 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090820 Year of fee payment: 10 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 11 Free format text: PAYMENT UNTIL: 20100820 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 12 Free format text: PAYMENT UNTIL: 20110820 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 12 Free format text: PAYMENT UNTIL: 20110820 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120820 Year of fee payment: 13 |
|
| EXPY | Cancellation because of completion of term | ||
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120820 Year of fee payment: 13 |