JPH04681B2 - - Google Patents
Info
- Publication number
- JPH04681B2 JPH04681B2 JP57184439A JP18443982A JPH04681B2 JP H04681 B2 JPH04681 B2 JP H04681B2 JP 57184439 A JP57184439 A JP 57184439A JP 18443982 A JP18443982 A JP 18443982A JP H04681 B2 JPH04681 B2 JP H04681B2
- Authority
- JP
- Japan
- Prior art keywords
- fluid
- outlet
- distance
- gap
- void
- 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
- 239000012530 fluid Substances 0.000 claims description 86
- 238000000926 separation method Methods 0.000 claims description 17
- 239000011800 void material Substances 0.000 claims description 12
- 238000005192 partition Methods 0.000 claims description 6
- 238000013459 approach Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 2
- 230000002093 peripheral effect Effects 0.000 claims 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 18
- 239000007788 liquid Substances 0.000 description 13
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000004587 chromatography analysis Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 229910021536 Zeolite Inorganic materials 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Description
【発明の詳細な説明】
本発明は充填塔に設置する流体分集装置の改良
に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an improvement in a fluid separation device installed in a packed column.
流体は充填塔内に流入あるいは充填塔外に流出
させる場合、流入させた液を充填物と接触させる
前に充填塔の半径方向に流体を、均一かつすみや
かに、できるだけ乱れを小さくして分散させた
り、充填物との接触が完了した液を、すみやか
に、できるだけ乱れを小さくして集液する装置が
必要となる。 When fluid flows into or out of a packed tower, the fluid must be dispersed uniformly and quickly in the radial direction of the packed tower with as little turbulence as possible before the inflowing liquid comes into contact with the packing. There is a need for a device that collects the liquid that has come into contact with the filling material quickly and with as little turbulence as possible.
また、特に、クロマトグラフイーにより物質を
分離することを目的とする充填塔においては、流
体の乱れによつて分離効率が大きく低下するた
め、上記のような流体分集装置を設置することが
非常に重要である。 In addition, especially in packed columns whose purpose is to separate substances by chromatography, the separation efficiency is greatly reduced due to fluid turbulence, so it is extremely difficult to install a fluid concentrator as described above. is important.
しかるに、従来の流体分集装置は、その構造が
複雑なものが多く、その部分で生じる流体の乱れ
が大きいという問題があつた。また、その構造が
簡単なものについては、流体の分集が満足のいく
ものではなく、流体分集装置内で流体の流れの時
間的な遅れが大きいという問題があつた。そのた
めに、例えば流体出口においては、充填物との接
触時間の異なる着目流体、あるいは充填塔内を流
れている他の流体との接触時間の異なる着目流体
が混合されるために見かけ上充填塔の性能が低下
していた。また、特にクロマトグラフイーにより
物質を分離することを目的とする充填塔において
は、上記現象のため流体に与える乱れが大きく、
分離効率の低下の一因となつていた。 However, many of the conventional fluid separation devices have complicated structures, and there is a problem in that large turbulence of the fluid occurs in these parts. Furthermore, with simple structures, the separation and concentration of the fluid was not satisfactory, and there was a problem that there was a large time delay in the flow of the fluid within the fluid separation device. For this reason, for example, at the fluid outlet, fluids of interest that have different contact times with the packing material or fluids that have different contact times with other fluids flowing in the packed column are mixed, so that the appearance of the packed column appears to be Performance was declining. In addition, especially in packed columns whose purpose is to separate substances by chromatography, the above phenomenon causes large turbulence to the fluid.
This was a contributing factor to the decrease in separation efficiency.
本発明者は、流体分集装置の構造を検討し、従
来のものよりも構造が簡単かつ安価でしかも流体
に与え乱れが従来のものよりも少ない流体分集装
置を開発すべく検討をすすめた結果、本発明をす
るに至つた。 The present inventor studied the structure of a fluid concentrator, and as a result of conducting studies to develop a fluid concentrator that is simpler and cheaper in structure than conventional ones, and causes less turbulence to the fluid than conventional ones, This led to the present invention.
すなわち、本発明の流体分集装置は、その内部
に空隙を有し、空隙を形成する２つの面：
Ａ面：流体は通過するが、充填物は通過しない
仕切板又はそれを支持するための多孔板の
端面で流体出入口に近い面
Ｂ面：流体出入口が接続されている固体部分で
Ａ面と相対している面
の構造が空隙の代表断面積の95％以上の範囲で流
体出入口から外周部にいたるすべての方向につい
てＡ面に対するＢ面の傾きが少なくとも１回変化
し、かつＡ面とＢ面の間隔が少なくとも増大する
ことがないことを特徴とする。 That is, the fluid collection device of the present invention has a void inside thereof, and has two surfaces forming the void: A surface: a partition plate through which the fluid passes but not the filler, or a porous hole for supporting it; Surface close to the fluid inlet/outlet on the end face of the plate Surface B: The solid part to which the fluid inlet/outlet is connected, and the structure of the surface facing A side is from the fluid inlet/outlet to the outer periphery within a range of 95% or more of the representative cross-sectional area of the void. The inclination of the B plane with respect to the A plane changes at least once in all directions up to , and the distance between the A plane and the B plane does not increase at least.
ここで「空隙の代表断面積」とは充填塔の横断
面と平行な空隙の断面のうち最大のものを示す。
ただし空隙の該断面の面積が充填塔の横断面の面
積よりも大きい場合には充填塔の横断面の面積を
空隙の代表断面積とする。また、ここで充填物を
塔内に保持するために用いられる仕切板として考
えられるものは多孔質の材料でできた板、多孔
板、金網、各種の織物、金属、有機物及び無機物
の焼結体等がある。更に、空隙を保つ方法として
は、上記仕切板自体による方法、仕切板を支持す
るための多孔板を設置する方法又は当該空隙内に
流体の流れにほとんど影響を与えないような目の
粗い金網、多孔質の材料製の板を設置して仕切板
を支える方法、空隙内に流体の流れに影響を与え
ない粒径のビーズを設置する方法、空隙内にＡ面
を支えるための柱を設置する方法等がある。 Here, the "representative cross-sectional area of the void" refers to the largest cross section of the void parallel to the cross section of the packed tower.
However, if the cross-sectional area of the void is larger than the cross-sectional area of the packed tower, the cross-sectional area of the packed tower is taken as the representative cross-sectional area of the void. In addition, possible partition plates used to retain the packing inside the tower include plates made of porous materials, perforated plates, wire mesh, various fabrics, metals, and sintered bodies of organic and inorganic materials. etc. Furthermore, the method of maintaining the gap includes the above-mentioned method using the partition plate itself, the method of installing a perforated plate to support the partition plate, or the method of using a coarse wire mesh that hardly affects the flow of fluid in the gap. A method is to install a plate made of porous material to support the partition plate, a method to install beads with a particle size that does not affect the flow of fluid in the gap, a method to install a pillar to support side A in the gap. There are methods etc.
本発明の流体分集装置のような構造にした場
合、流体の流量が流体出入口近傍よりも少ない空
隙内の外周部近傍でＡ，B2面間の間隔が小さく
なるため、流体の流速が小となることがなくな
り、外周部での流体の流れの時間的な遅れを少な
くすることが可能となる。 When a structure like the fluid concentrator of the present invention is adopted, the gap between the two surfaces A and B becomes smaller near the outer periphery in the gap where the fluid flow rate is lower than near the fluid inlet/outlet, so the fluid flow velocity becomes small. Therefore, it is possible to reduce the time delay in the flow of fluid at the outer circumference.
また、Ｂ面が１つの傾きしか持たず、かつ中心
部に近づくにつれＡ，Ｂ両面間の間隔が大きくな
るようなテーパーを有する場合に比較して中心付
近のＡ，B2面間の間隔を同じにした場合、本発
明の流体分集装置の方が外周部近傍でＡ，B2面
間の間隔が極端に小となる部分を少なくすること
が可能なため、流体が流れ難い部分を少なくする
ことができ、スムーズな流れを実現することが可
能となる。 Also, compared to the case where the B side has only one inclination and has a taper where the distance between both surfaces A and B increases as it approaches the center, the distance between the two surfaces A and B near the center is the same. In this case, the fluid concentrator of the present invention can reduce the part where the distance between the two surfaces A and B is extremely small near the outer periphery, so it can reduce the part where the fluid has difficulty flowing. This makes it possible to realize a smooth flow.
本発明の流体分集装置のより好ましい構造は以
下の通りであり、このような構造にすることによ
り、流体分集装置をより簡単かつ安価に製作する
ことが可能である。その構造とは空隙内のＡ，
B2つの面のうちＢ面が外周に近づくにつれＡ，
B2面間の間隔が小とするような構造を有する部
分とその内側のＡ，B2面間の間隔が一定である
構造を有する部分とから成るものである。 A more preferable structure of the fluid separating device of the present invention is as follows, and by adopting such a structure, it is possible to manufacture the fluid separating device more easily and at low cost. The structure is A in the void,
BAs the B side approaches the outer periphery of the two surfaces, A,
It consists of a part having a structure in which the distance between the B2 surfaces is small, and an inner part having a structure in which the distance between the A and B2 surfaces is constant.
更に、本発明の流体分集装置において、外周部
におけるＡ，B2面間の間隔が該空隙内での最小
値であり、かつ、その値が0.5mm以上であること
が望ましい。このような構造にした場合、外周部
においても空隙の間隔が０の部分がなくなるた
め、外周部における液の流れはよりスムーズにな
り、空隙内で流体に与える乱れをより少なくする
ことが可能となる。 Furthermore, in the fluid concentrator of the present invention, it is preferable that the distance between the two surfaces A and B at the outer periphery is the minimum value within the gap, and that value is 0.5 mm or more. With such a structure, there is no part where the gap between gaps is 0 at the outer periphery, so the flow of liquid at the outer periphery becomes smoother, and it is possible to further reduce the turbulence given to the fluid within the gaps. Become.
特に充填塔内の流体の流量が高い場合、あるい
は充填塔の径を大型化し、塔内をスケールアツプ
以前と同一線速度で流体を流そうとする場合、流
体分集装置の空隙の流体入口あるいは出口の近傍
での流量が増大するために局部的に流体が流れ難
くなつたり、流体入口の場合、流体が配管から吹
き出す流速が高くなり、Ａ面に衝突した時にその
部分で特異的に流体の突抜け現象が生じその面の
直下の充填層でその部分のみが高流速で流れると
いう問題が生じる。このような場合には流体分集
装置の空隙の流体の入口あるいは出口近傍におい
て入口あるいは出口に近づくにつれ、空隙の間隔
が大となるようなテーパーをつけ（テーパーをつ
けることにより流体入口あるいは出口の管径を大
とすることになる）中心部の流体の線速度を減少
させることが好ましい。 Especially when the flow rate of the fluid in the packed tower is high, or when the diameter of the packed tower is increased and the fluid is to flow at the same linear velocity as before scale-up, the fluid inlet or outlet of the gap in the fluid concentrator The flow rate increases near the A surface, making it difficult for the fluid to flow locally, or in the case of a fluid inlet, the flow velocity of fluid blowing out of the piping increases, causing a specific fluid bulge in that part when it collides with the A side. A problem arises in which a shedding phenomenon occurs and only that portion of the packed bed directly below that surface flows at a high flow rate. In such a case, the gap in the fluid concentrator should be tapered near the fluid inlet or outlet so that the gap between the gaps becomes larger as it approaches the inlet or outlet. It is preferable to reduce the linear velocity of the fluid in the center (which would increase the diameter).
更に、本流体分集装置において、Ｄとlsavから
以下のように定義されるｋ値
ｋ＝lsav／D2/3
が0.01≦ｋ≦0.04であれば、流体が流体分集装置
を通過する際に生じる乱れを少なくすることがで
き好ましい。 Furthermore, in this fluid concentrator, if the k value defined from D and lsav as follows: k = lsav/D 2/3 is 0.01≦k≦0.04, then this occurs when the fluid passes through the fluid concentrator. This is preferable because it can reduce disturbance.
上記式において
lsav＝（r2−r1）×ls＋（r3−r2）×（ls
2＋lt）／２／r3−r1
（r1，r2，r3，ls1，ls2，ltは第１図参照）
Ｄ＝充填塔の内径〔cm〕を示す。 In the above formula, lsav = (r 2 − r 1 ) × ls + (r 3 − r 2 ) × (ls
2 + lt)/2/r 3 - r 1 (r 1 , r 2 , r 3 , ls 1 , ls 2 , lt refer to Figure 1) D = indicates the inner diameter of the packed column [cm].
上記ｋの値が上記範囲より大の場合には流体分
集装置の空隙体積が大きくなり、流体が空隙内を
通過する際に生じる乱れが大となりかつ流体の流
れの塔内横断面図の位置とする時間的な遅れが大
となる傾向があるので好ましくない。またｋの値
が上記の範囲より小の場合には、流体分集装置内
の流体の流れが不均一となつたり、空隙を形成し
ているＡ，B2つの面の若干の変形により空隙内
を流れる流体の流れ状態が大きく変化するために
安定した性能が得られなくなる傾向にあるので好
ましくない。 If the value of k is larger than the above range, the pore volume of the fluid concentrator becomes large, the turbulence generated when the fluid passes through the pores becomes large, and the position of the fluid flow in the cross-sectional view of the tower increases. This is undesirable because it tends to cause a large time delay. In addition, if the value of k is smaller than the above range, the fluid flow within the fluid collector may become uneven, or the fluid may flow within the gap due to slight deformation of the two surfaces A and B forming the gap. This is not preferable because stable performance tends not to be obtained due to large changes in the fluid flow state.
特にクロマトグラフイーにより物質を分離する
ことを目的とした充填塔においては、流体の乱れ
が分離効率に大きく影響するため上記ｋの範囲を
0.015≦ｋ≦0.03
とすることが好ましい。 In particular, in a packed column intended for separating substances by chromatography, the turbulence of the fluid greatly affects the separation efficiency, so it is preferable that the range of k be 0.015≦k≦0.03.
本発明の流体分集装置において第１図上のr3×
２とＤが等しい必要はないが、Ｄの15％以内の範
囲でr3×２とＤが一致することにより空隙外周部
近傍で液だまりが生じたり、流体の分集が不完全
となることが少なくなり、結果的に空隙内を通過
する際に生じる流体の乱れを少なくできるため好
ましい。 In the fluid concentrator of the present invention, r 3 × on FIG.
2 and D do not have to be equal, but if r 3 × 2 and D match within 15% of D, a pool of liquid may occur near the outer periphery of the gap or the distribution of fluid may be incomplete. This is preferable because the turbulence of the fluid that occurs when passing through the gap can be reduced.
次に実施例及び比較例を示して本発明を説明す
る。例中、流れの均一性を示す指標として、非対
称係数FTを用いた。この係数FTは、次のような
ものである。 Next, the present invention will be explained by showing examples and comparative examples. In the example, the asymmetry coefficient F T was used as an indicator of flow uniformity. This coefficient F T is as follows.
充填塔内に0.1N塩酸を一定流量で流しながら、
塔入口直前に設けた液注入口より、2M／食塩
水を一定微少量注入し、排出する液を分取した
後、Na濃度を原子吸光分析装置を用いて測定し、
横軸に2M／食塩水を注入してからの排出液量
を、縦軸に排出液のNa濃度をプロツトしてパル
ス波形を得、その形状を調べる。 While flowing 0.1N hydrochloric acid at a constant flow rate into the packed column,
A constant, minute amount of 2M saline was injected through the liquid injection port provided just before the tower entrance, and the discharged liquid was collected, and the Na concentration was measured using an atomic absorption spectrometer.
Plot the amount of liquid drained after injecting 2M/saline on the horizontal axis and the Na concentration of the drained liquid on the vertical axis to obtain a pulse waveform and examine its shape.
流体分集装置の性能が悪い場合には、流体分集
装置内で流体の流れの時間的な遅れが生じるた
め、出口でのパルス波形は、より大きなテーリン
グを生じる傾向を示す。従つて、このテーリング
の差を表す尺度としてパルスの非対称係数を用い
た。 When the performance of the fluid concentrator is poor, the pulse waveform at the outlet tends to exhibit greater tailing due to the time delay of the fluid flow within the fluid concentrator. Therefore, the pulse asymmetry coefficient was used as a measure of the difference in tailing.
パルスの非対称係数FTとは、パルスのピーク
高さの１／10におけるピーク位置より前のパルス
の幅（WF）に対する、ピーク位置から後のパル
スの幅（WR）の比である。 The pulse asymmetry coefficient F T is the ratio of the width of the pulse after the peak position (W R ) to the width of the pulse before the peak position (W F ) at 1/10 of the peak height of the pulse.
FT＝WR／WF
このFT値が１より大きければ大きい程テーリ
ングの度合が激しいこと、即ち、流れの不均一性
の大きいことを示す。 F T =W R /W F The larger the F T value is than 1, the more severe the tailing is, that is, the greater the non-uniformity of the flow.
実施例 １
内径30cm、長さ50cmの充填塔の上下に第１図に
示す構造の流体分集装置をＡ面が塔の内部になる
様に設置した充填塔を用意した。ここで流体分集
装置の各部分の長さは、r1＝30mm、r2＝75mm、r3
＝150mm、lc＝10mm、ls1＝ls2＝2.5mm、lt0.5mmであ
つた。Example 1 A packed tower having an inner diameter of 30 cm and a length of 50 cm was provided with fluid collectors having the structure shown in FIG. 1 installed above and below the tower so that side A was inside the tower. Here, the length of each part of the fluid collector is r 1 = 30 mm, r 2 = 75 mm, r 3
= 150 mm, lc = 10 mm, ls 1 = ls 2 = 2.5 mm, l t 0.5 mm.
また、Ａ面は平均孔径40μで長さ３mmテフロン
フイルターを用い、空隙を保つために空隙内に50
メツシユの金網を設置した。 In addition, for side A, a Teflon filter with an average pore diameter of 40μ and a length of 3mm was used, and in order to maintain the voids, 50μ
A mesh wire fence was installed.
以上の様な装置に、スチレン−ジビニルベンゼ
ン共重合物をクロロメチル化した後にトリメチル
アミンで四級アンモニウム化した陰イオン交換樹
脂のCl型であつて0.26gr乾燥樹脂／c.c.湿潤樹脂、
架橋度８％、粒径100〜200メツシユの樹脂を塔の
上部迄充填した。 In the above apparatus, 0.26 gr dry resin/cc wet resin, which is a Cl type anion exchange resin made by chloromethylating a styrene-divinylbenzene copolymer and then quaternary ammonium using trimethylamine, was installed.
A resin having a degree of crosslinking of 8% and a particle size of 100 to 200 mesh was filled to the top of the tower.
イオン交換樹脂の充填は塔上部の流体分集装置
を外した状態で行ない、充填終了後流体分集装置
を設置し以下の様な実験を行なつた。すなわち
0.1N塩酸溶液を7.2／分の速度で流しながら塔
入口直前に設けた液注入口より2M／の塩化ナ
トリウム溶液0.2mlを瞬間的に注入し、塔出口か
ら流出する液を50mlのフラクシヨンに分けて採取
し、原子吸光分析装置により各フラクシヨン中の
ナトリウム濃度を測定した。これらの測定値を横
軸に流出液量、縦軸にナトリウム濃度をプロツト
してパルス波形を得た。非対称係数は1.18であつ
た。 Filling with ion exchange resin was carried out with the fluid collector at the top of the column removed, and after the filling was completed, the fluid collector was installed and the following experiments were conducted. i.e.
While flowing 0.1N hydrochloric acid solution at a rate of 7.2 min, 0.2 ml of 2 M sodium chloride solution was instantaneously injected from the liquid inlet provided just before the tower inlet, and the liquid flowing out from the tower outlet was divided into 50 ml fractions. The sodium concentration in each fraction was measured using an atomic absorption spectrometer. These measured values were plotted with the effluent volume on the horizontal axis and the sodium concentration on the vertical axis to obtain a pulse waveform. The asymmetry coefficient was 1.18.
比較例 １
実施例１の装置で、流体分集装置を第２図に示
すものに変えただけの充填塔を用意し、同様の操
作を行なつた。第２図で各部の長さはls＝３mm、
r2＝150mmであつた。非対称係数は1.4であつた。Comparative Example 1 A packed column was prepared by using the apparatus of Example 1 except that the fluid separation device was changed to that shown in FIG. 2, and the same operation was performed. In Figure 2, the length of each part is ls = 3mm,
r 2 =150 mm. The asymmetry coefficient was 1.4.
実施例 ２
内径10cm、長さ30cmの充填塔の上下に第１図に
示す構造の流体分集装置をＡ面が塔の内部になる
様に設置した充填塔を用意した。ここで流体分集
装置の各部分の長さはr1＝０mm、r2＝25mm、lc＝
ls1＝ls2＝1.5mmlt＝２mmであつた。Ａ面の材質及
び空隙を保つための構造は実施例１と同じであ
る。Example 2 A packed tower having an inner diameter of 10 cm and a length of 30 cm was provided with fluid collectors having the structure shown in FIG. 1 installed above and below the tower so that side A was located inside the tower. Here, the length of each part of the fluid concentrator is r 1 = 0 mm, r 2 = 25 mm, lc =
ls 1 = ls 2 = 1.5 mmlt = 2 mm. The material of the A side and the structure for maintaining the gap are the same as in Example 1.
実施例１と同様の実験を0.1N塩酸溶液の流量
を0.8／min各フラクシヨンの液量を５mlにし
て行なつた結果、得られたパルス波形の非対称係
数は1.1であつた。 The same experiment as in Example 1 was carried out with the flow rate of 0.1N hydrochloric acid solution being 0.8/min and the liquid volume of each fraction being 5 ml. As a result, the asymmetry coefficient of the obtained pulse waveform was 1.1.
実施例 ３
内径100cm、長さ80cmの充填塔の上下に第１図
に示す構造の流体分集装置をＡ面が塔の内部にな
る様に設置した充填塔を用意した。ここで流体分
集装置の各部分の長さは、r1＝50mm、r2＝25mm、
r3＝500mm、lc＝20mm、ls1＝ls2＝６mm、lt＝２mm
であつた。Ａ面の材質及び空隙を保つための構造
は実施例１と同じとした。Example 3 A packed tower having an inner diameter of 100 cm and a length of 80 cm was prepared, in which fluid collectors having the structure shown in FIG. 1 were installed above and below the tower so that side A was located inside the tower. Here, the length of each part of the fluid collector is r 1 = 50 mm, r 2 = 25 mm,
r 3 = 500mm, lc = 20mm, ls 1 = ls 2 = 6mm, lt = 2mm
It was hot. The material of side A and the structure for maintaining voids were the same as in Example 1.
実施例１と同様の検討を0.1N塩酸溶液の流量
を80／min各フラクシヨンの液量を500mlにし
て行なつた結果、得られたパルス波形の非対称係
数は1.23であつた。 The same study as in Example 1 was conducted using a flow rate of 0.1N hydrochloric acid solution of 80/min and a liquid volume of each fraction of 500 ml. As a result, the asymmetry coefficient of the obtained pulse waveform was 1.23.
実施例 ４
内径300mm、長さ1000mmのジヤケツト付クロマ
トカラムに実施例１で使用した流体分集装置を設
置し、この分離塔にゼオライト（60〜100メツシ
ユ）を充填した。Example 4 The fluid separation device used in Example 1 was installed in a jacketed chromatography column with an inner diameter of 300 mm and a length of 1000 mm, and this separation column was filled with zeolite (60 to 100 mesh).
ゼオライトを充填し終つたカラムを温度100℃
に保ち、先ずトルエンを供給してゼオライトをコ
ンデイシヨニングし、ついで被分離物質としてベ
ンゼン50重量％、シクロヘキセン32.5重量％、シ
クロヘキサン17.5重量％からなるC6混合物23.4
を定量ポンプにて供給しC6混合物吸着帯を形成
した。その後再びトルエンをカラムに8.4／分
の一定流速で供給し、C6混合物吸着帯を展開し
た。カラム底部より流出する溶離液を0.25〜2.5
ずつのフラクシヨンに分割して採取した。この
ようにして採取したサンプル液のベンゼン、シク
ロヘキセン、シクロヘキサン、トルエンの重量％
をガスクロマトグラフイーにより定量分析した。 After filling the column with zeolite, the temperature is 100℃.
First, toluene is supplied to condition the zeolite, and then a 23.4% C6 mixture consisting of 50% by weight of benzene, 32.5% by weight of cyclohexene, and 17.5% by weight of cyclohexane is added as the substance to be separated.
was supplied using a metering pump to form a C6 mixture adsorption zone. Thereafter, toluene was again supplied to the column at a constant flow rate of 8.4/min to develop a C6 mixture adsorption zone. The eluent flowing out from the bottom of the column is 0.25 to 2.5
It was divided into different fractions and collected. Weight percentage of benzene, cyclohexene, cyclohexane, and toluene in the sample liquid collected in this way
was quantitatively analyzed by gas chromatography.
溶離液の進行方向に対してC6混合物吸着帯の
前端界面近傍より、シクロヘキセン及びシクロヘ
キサンに富んだ溶液が、また後端界面近からはベ
ンゼンに富んだ液が回収された。分離効率の目安
として、ベンゼンのC6混合物に対する純度が99
％以上であるフラクシヨンに含まれるベンゼンの
重量は5.13Kgであつた。 A solution rich in cyclohexene and cyclohexane was recovered from near the front interface of the C6 mixture adsorption zone in the direction of movement of the eluent, and a solution rich in benzene was recovered from near the rear interface. As a guideline for separation efficiency, the purity of benzene for C6 mixture is 99
The weight of benzene contained in the fraction was 5.13 kg.
比較例 ２
内径300cm、長さ1000cmのジヤケツト付クロマ
トカラムに比較例１で使用した流体分集装置を設
置した分離塔を用意し、これに実施例３と同じゼ
オライトを充填し、実施例３と同様の操作により
分離を行なつた。Comparative Example 2 A separation column was prepared in which a jacketed chromatography column with an inner diameter of 300 cm and a length of 1000 cm was installed with the fluid separator used in Comparative Example 1, and the same zeolite as in Example 3 was packed in it. Separation was performed by the following procedure.
その結果、混合物に対する純度が99％以上であ
るフラツクシヨンに含まれるベンゼンの重量は
4.11Kgに過ぎなかつた。 As a result, the weight of benzene contained in the fraction with a purity of 99% or higher relative to the mixture is
It weighed only 4.11Kg.
第１図は実施例において使用した本発明に従つ
た流体分集装置の一例を示す断面図であり、第２
図は比較例において使用した流体分集装置の一例
を示す断面である。
１及び４……流体出入口、２及び５……Ａ面、
３及び６……Ｂ面。
FIG. 1 is a sectional view showing an example of a fluid concentrator according to the present invention used in Examples;
The figure is a cross section showing an example of a fluid separation device used in a comparative example. 1 and 4...Fluid inlet/outlet, 2 and 5...A side,
3 and 6... Side B.
Claims (1)
に空隙を有し、空隙を形成する２つの面： Ａ面：流体は通過するが、充填物は通過しない
仕切板又はそれを支持するための多孔板の
端面で流体出入口に近い面 Ｂ面：流体出入口が接続されている固体部分で
Ａ面と相対している面 の構造が空隙の代表断面積の95％以上の範囲で流
体の出入口から外周部にいたるすべての方向につ
いてＡ面に対するＢ面の傾きが少なくとも１回変
化し、かつＡ面とＢ面の間隔が少なくとも増大す
ることがないような構造であることを特徴とする
改良型流体分集装置。 ２ 空隙を形成するＡ，B2つの面のうちＢ面が
外周に近づくにつれＡ，B2面間の間隔が小とな
るような構造を有する部分とその内側のＡ，B2
面間の間隔が一定である構造を有する特許請求の
範囲第１項に記載の装置。 ３ 空隙内の外周部において、Ａ，B2面間の間
隔が該空隙内で最小値であり、その値が0.5mm以
上である特許請求の範囲第１項又は第２項に記載
の装置。 ４ 流体分集装置の流体出入口近傍おいて、流体
出入口に近づくにつれＡ，B2面間の間隔が大と
なるようなテーパーを有する構造をもつ特許請求
の範囲第１項〜第３項のいずれか１項に記載の装
置。 ５ 充填塔の内径Ｄ（cm）と空隙内のＡ，B2面間
の平均間隔（但し中心部は除く）lsav（cm）で以
下のように定義されるｋ値 ｋ＝lsav／D2/3 が0.01≦ｋ≦0.04である特許請求の範囲第１項〜
第４項のいずれか１項に記載の装置。[Claims] 1. A fluid separation device installed in a packed tower, which has a void inside and has two surfaces forming the void: A surface: a partition plate or The end face of the perforated plate for supporting it, which is close to the fluid inlet/outlet. Surface B: The solid part to which the fluid inlet/outlet is connected, and the structure of the surface facing A side is larger than 95% of the representative cross-sectional area of the void. The structure is such that the inclination of the B plane with respect to the A plane changes at least once in all directions from the fluid inlet and outlet to the outer periphery, and the distance between the A plane and the B plane does not increase at least. Improved fluid separation device featuring features. 2 Among the two surfaces A and B that form the gap, the part that has a structure in which the distance between the two surfaces A and B becomes smaller as the B surface approaches the outer periphery, and the A and B2 inside thereof
2. The device according to claim 1, having a structure in which the spacing between surfaces is constant. 3. The device according to claim 1 or 2, wherein the distance between the two planes A and B is the minimum value within the gap, and that value is 0.5 mm or more at the outer peripheral portion of the gap. 4. Any one of claims 1 to 3 having a tapered structure near the fluid inlet/outlet of the fluid separation device such that the distance between the two surfaces A and B increases as the distance approaches the fluid inlet/outlet. The equipment described in section. 5 The k value defined as below by the inner diameter D (cm) of the packed tower and the average distance between the A and B planes in the void (excluding the center) lsav (cm) k = lsav/D 2/3 Claims 1 to 0.01≦k≦0.04
Apparatus according to any one of clause 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57184439A JPS5976503A (en) | 1982-10-22 | 1982-10-22 | Fluid collector of improved type |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57184439A JPS5976503A (en) | 1982-10-22 | 1982-10-22 | Fluid collector of improved type |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5976503A JPS5976503A (en) | 1984-05-01 |
| JPH04681B2 true JPH04681B2 (en) | 1992-01-08 |
Family
ID=16153168
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57184439A Granted JPS5976503A (en) | 1982-10-22 | 1982-10-22 | Fluid collector of improved type |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5976503A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63179250A (en) * | 1987-01-21 | 1988-07-23 | Hitachi Ltd | Column for liquid chromatography |
-
1982
- 1982-10-22 JP JP57184439A patent/JPS5976503A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5976503A (en) | 1984-05-01 |
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