JPH06254355A - Separation - Google Patents
SeparationInfo
- Publication number
- JPH06254355A JPH06254355A JP7123993A JP7123993A JPH06254355A JP H06254355 A JPH06254355 A JP H06254355A JP 7123993 A JP7123993 A JP 7123993A JP 7123993 A JP7123993 A JP 7123993A JP H06254355 A JPH06254355 A JP H06254355A
- Authority
- JP
- Japan
- Prior art keywords
- hollow fiber
- fiber membrane
- membrane module
- potting
- potting agent
- 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.)
- Withdrawn
Links
- 238000000926 separation method Methods 0.000 title claims abstract description 30
- 239000012528 membrane Substances 0.000 claims abstract description 114
- 239000012510 hollow fiber Substances 0.000 claims abstract description 111
- 238000004382 potting Methods 0.000 claims abstract description 40
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000005373 pervaporation Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims description 33
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 6
- 238000005336 cracking Methods 0.000 abstract description 8
- 238000007789 sealing Methods 0.000 abstract description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 15
- 238000000605 extraction Methods 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- 239000012466 permeate Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229920002492 poly(sulfone) Polymers 0.000 description 2
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
(57)【要約】
【目的】中空糸膜モジュールを構成するポッテイング材
のひび割れを防止し、長時間の連続運転を行い得るよう
に改良された浸透気化による分離方法を提供する。
【構成】中空糸膜モジュールを用いた浸透気化による分
離方法において、中空糸膜モジュールとして、多数の中
空糸膜（１）が束状に引き揃えられ、その両端がポッテ
イング剤（２）、（３）で相互に固定され、一端側の各
中空糸膜（１）の先端がポッテイング剤の端面に露出し
て開口端（４）を形成し、他端側の各中空糸膜（１）の
先端がポッテイング剤中に埋没されて封止端（５）を形
成して成る中空糸膜モジュールを用い、そして、中空糸
膜（１）の内側を減圧状態とすることにより、中空糸膜
（１）の外側から内側に透過成分を移動させる。
(57) [Summary] [Object] To provide a separation method by pervaporation which is improved so as to prevent cracking of the potting material constituting the hollow fiber membrane module and to allow continuous operation for a long time. In a separation method by pervaporation using a hollow fiber membrane module, as a hollow fiber membrane module, a large number of hollow fiber membranes (1) are aligned in a bundle, and both ends thereof are potting agents (2), (3). ), The ends of the hollow fiber membranes (1) on one end side are exposed at the end face of the potting agent to form open ends (4), and the ends of the hollow fiber membranes (1) on the other end side are A hollow fiber membrane module (1) is used in which a hollow fiber membrane module is formed by burying a hollow fiber in a potting agent to form a sealing end (5), and by making the inside of the hollow fiber membrane (1) under reduced pressure. The transmitted component is moved from the outside to the inside.
Description
【０００１】[0001]
【産業上の利用分野】本発明は、分離方法に関するもの
であり、詳しくは、中空糸膜モジュールを用いた浸透気
化による分離方法であって、中空糸膜モジュールを構成
するポッテイング剤（固着剤）のひび割れを防止し、長
時間の連続運転を行い得るように改良された分離方法に
関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a separation method, and more particularly to a separation method by pervaporation using a hollow fiber membrane module, which is a potting agent (fixing agent) constituting the hollow fiber membrane module. The present invention relates to an improved separation method capable of preventing cracking of the steel and allowing continuous operation for a long time.
【０００２】[0002]
【従来の技術】分離膜を用いた分離方法として浸透気化
法が知られている。浸透気化法は、混合液体中の特定成
分と親和性を有する分離膜を利用し、分離膜の１方側
（１次側）に混合液体を供給し、他方側（２次側）を減
圧にするか、または、不活性ガスで掃気することによ
り、２次側における透過成分の蒸気分圧を１次側の平衡
蒸気圧よりも小さい値に保持して特定成分を他方側に通
過させて分離を行う方法である。例えば、分離対象液が
水溶性有機溶剤と水との混合液体であり、分離膜が水と
親和性を有する場合は、水を透過させて濃縮分離するこ
とが出来る。2. Description of the Related Art A pervaporation method is known as a separation method using a separation membrane. The pervaporation method utilizes a separation membrane having an affinity for a specific component in the mixed liquid, supplies the mixed liquid to one side (primary side) of the separation membrane, and depressurizes the other side (secondary side). Or by purging with an inert gas, the vapor partial pressure of the permeated component on the secondary side is kept at a value smaller than the equilibrium vapor pressure on the primary side and the specific component is passed to the other side for separation. Is the way to do. For example, when the liquid to be separated is a mixed liquid of a water-soluble organic solvent and water, and the separation membrane has an affinity for water, the water can be permeated and concentrated.
【０００３】また、浸透気化法に用いる分離膜の一つと
して中空糸膜モジュールが知られている。図４は、中空
糸膜モジュールを用いた浸透気化による従来の分離方法
の説明図である。中空糸膜モジュールは、多数の中空糸
膜（１）が束状に引き揃えられ、その両端がポッテイン
グ剤（２）、（３）で相互に固定され、両端側の各中空
糸膜（１）の先端がポッテイング剤の端面に露出して開
口端（４）、（４）を形成して構成される。中空糸膜
（１）は、分離機能を有する材料にて成形された外径
０．５〜２．０ｍｍ程度のストロー状の中空糸であり、
通常、数十〜数万本束ねて用いられる。A hollow fiber membrane module is known as one of the separation membranes used in the pervaporation method. FIG. 4 is an explanatory diagram of a conventional separation method by pervaporation using a hollow fiber membrane module. In the hollow fiber membrane module, a large number of hollow fiber membranes (1) are aligned in a bundle, and both ends thereof are fixed to each other with potting agents (2) and (3), and the hollow fiber membranes (1) on both end sides are arranged. Is exposed at the end surface of the potting agent to form open ends (4) and (4). The hollow fiber membrane (1) is a straw-shaped hollow fiber formed of a material having a separating function and having an outer diameter of about 0.5 to 2.0 mm.
Usually, tens to tens of thousands are used in a bundle.
【０００４】中空糸膜モジュールは、両側にそれぞれ原
料供給口（６）と非透過液抜き出し口（７）を備え、中
間部に透過蒸気抜き出し口（８）を備えたたハウジング
（９）内に収納され、Ｏリング（１０）により両端でシ
ールされている。中空糸膜（１）の２次側（中空糸膜の
外側）は、透過蒸気抜き出し口（８）側に接続された真
空ポンプ（図示せず）により減圧にされる。分離対象液
は、原料供給口（６）から中空糸膜（１）の内側に供給
され、非透過成分は、中空糸膜（１）の内側を流れて非
透過液抜き出し口（７）から抜き出される。気化して中
空糸膜（１）を透過した透過成分は、透過蒸気抜き出し
口（８）から抜き出され、凝縮器（図示せず）で液化さ
れる。The hollow fiber membrane module has a housing (9) having a raw material supply port (6) and a non-permeate extraction port (7) on both sides and a permeated vapor extraction port (8) in the middle. It is stored and sealed at both ends by O-rings (10). The secondary side of the hollow fiber membrane (1) (outside the hollow fiber membrane) is decompressed by a vacuum pump (not shown) connected to the permeated vapor extraction port (8) side. The liquid to be separated is supplied from the raw material supply port (6) to the inside of the hollow fiber membrane (1), and the non-permeable component flows inside the hollow fiber membrane (1) and is extracted from the non-permeable liquid extraction port (7). Will be issued. The permeated component that has been vaporized and permeated through the hollow fiber membrane (1) is extracted from the permeated vapor extraction port (8) and liquefied by a condenser (not shown).
【０００５】[0005]
【発明が解決しようとする課題】浸透気化用中空糸膜モ
ジュールとして、中空糸膜（１）の先端を両側とも開口
させた中空糸膜モジュールによる従来の分離方法は、し
ばしば、ポッテイング剤（２）、（３）にひび割れが発
生し、長時間の連続運転が出来ないと言う問題がある。
斯かるひび割れ現象は、本発明者等の知見によれば、中
空糸膜（１）の内側に供給された分離対象液によって中
空糸膜（１）が膨潤することにより起こると考えられ
る。本発明は、上記実情に鑑みなされたものであり、そ
の目的は、中空糸膜モジュールを構成するポッテイング
剤のひび割れを防止し、長時間の連続運転を行い得るよ
うに改良された浸透気化による分離方法を提供すること
にある。As a hollow fiber membrane module for pervaporation, a conventional separation method using a hollow fiber membrane module in which both ends of the hollow fiber membrane (1) are opened is often a potting agent (2). , (3) is cracked, and there is a problem that continuous operation cannot be performed for a long time.
According to the findings of the present inventors, such a cracking phenomenon is considered to be caused by the swelling of the hollow fiber membrane (1) by the liquid to be separated supplied to the inside of the hollow fiber membrane (1). The present invention has been made in view of the above situation, and an object thereof is to prevent cracking of a potting agent that constitutes a hollow fiber membrane module and improve separation by pervaporation so that continuous operation for a long time can be performed. To provide a method.
【０００６】[0006]
【課題を解決するための手段】すなわち、本発明の要旨
は、中空糸膜モジュールを用いた浸透気化による分離方
法において、中空糸膜モジュールとして、多数の中空糸
膜（１）が束状に引き揃えられ、その両端がポッテイン
グ剤（２）、（３）で相互に固定され、一端側の各中空
糸膜（１）の先端がポッテイング剤の端面に露出して開
口端（４）を形成し、他端側の各中空糸膜（１）の先端
がポッテイング剤中に埋没されて封止端（５）を形成し
て成る中空糸膜モジュールを用い、そして、中空糸膜
（１）の内側を減圧状態とすることにより、中空糸膜
（１）の外側から内側に透過成分を移動させることを特
徴とする分離方法に存する。That is, the gist of the present invention is that in a separation method by pervaporation using a hollow fiber membrane module, a large number of hollow fiber membranes (1) are pulled in a bundle as a hollow fiber membrane module. Aligned, both ends thereof are fixed to each other with potting agents (2) and (3), and the tips of the hollow fiber membranes (1) on one end side are exposed at the end surface of the potting agent to form open ends (4). , A hollow fiber membrane module in which the tip of each hollow fiber membrane (1) on the other end side is embedded in a potting agent to form a sealing end (5), and the inside of the hollow fiber membrane (1) is used. In the separation method, the permeation component is moved from the outside to the inside of the hollow fiber membrane (1) by reducing the pressure.
【０００７】以下、本発明を詳細に説明する。図１は、
本発明の分離方法に用いられる中空糸膜モジュールの一
例の模式的断面説明図、図２は、図１のＡ−Ａ線の断面
図、図３は、本発明の分離方法を示す説明図であって、
浸透気化用中空糸膜モジュールをハウジングに収納した
状態の模式的断面説明図である。The present invention will be described in detail below. Figure 1
The typical cross section explanatory drawing of an example of the hollow fiber membrane module used for the separation method of this invention, FIG. 2: is sectional drawing of the AA line of FIG. 1, FIG. 3: is explanatory drawing which shows the separation method of this invention. There
It is a typical cross-section explanatory drawing of the state which accommodated the permeation | evaporation hollow fiber membrane module in the housing.
【０００８】本発明において、中空糸膜モジュールは、
多数の中空糸膜（１）が束状に引き揃えられ、その両端
がポッテイング剤（２）、（３）で相互に固定され、一
端側における各中空糸膜（１）の先端がポッテイング剤
の端面に露出して開口端（４）を形成し、他端側におけ
る各中空糸膜（１）の先端がポッテイング剤中に埋没さ
れて封止端（５）を形成して構成される。In the present invention, the hollow fiber membrane module is
A large number of hollow fiber membranes (1) are aligned in a bundle, both ends of which are fixed to each other by potting agents (2) and (3), and the tip of each hollow fiber membrane (1) on one end side is made of potting agent. An open end (4) is formed by being exposed on the end face, and the tip of each hollow fiber membrane (1) on the other end side is embedded in a potting agent to form a sealing end (5).
【０００９】中空糸膜（１）は、分離機能を有する材料
にて成形された外径０．５〜２．０ｍｍ程度のストロー
状の中空糸であり、通常、数十〜数万本束ねて用いられ
る。中空糸膜（１）の素材としては、浸透気化膜に用い
られる公知の材料から適宜選択できる。そして、本発明
において、中空糸膜（１）の素材は、分離機能を有する
限り、何ら制限されず、分離対象液によって膨潤する素
材をも選択することが出来、斯かる素材にて中空糸膜
（１）を形成した場合に本発明の利点は顕著である。The hollow fiber membrane (1) is a straw-shaped hollow fiber formed of a material having a separating function and having an outer diameter of about 0.5 to 2.0 mm, and usually bundles several tens to several tens of thousands. Used. The material of the hollow fiber membrane (1) can be appropriately selected from known materials used for pervaporation membranes. In the present invention, the material of the hollow fiber membrane (1) is not limited as long as it has a separating function, and a material that swells with the liquid to be separated can be selected. The advantage of the present invention is remarkable when (1) is formed.
【００１０】本発明において、分離対象液によって膨潤
する素材は、室温で分離対象液に浸漬した際に長手軸方
向に０．５％以上伸びる素材と定義される。そして、例
えば、分離対象液が水溶性有機溶剤と水との混合液体で
あり、水溶性有機溶剤がアルコール、ケトン等の場合
は、分離対象液によって膨潤する素材の具体例として、
ポリスルホン、ポリスルホンエーテル、ポリイミド、ポ
リアミド、ポリアクリロニトリル、セルロース等の樹脂
を例示することが出来る。また、このような樹脂によれ
ば、水を選択的に透過させる中空糸膜を容易に形成する
ことが出来る。In the present invention, a material that swells with a liquid to be separated is defined as a material that extends 0.5% or more in the longitudinal axis direction when immersed in the liquid to be separated at room temperature. Then, for example, the liquid to be separated is a mixed liquid of a water-soluble organic solvent and water, when the water-soluble organic solvent is alcohol, ketone, etc., as a specific example of the material swelling by the liquid to be separated,
Examples thereof include resins such as polysulfone, polysulfone ether, polyimide, polyamide, polyacrylonitrile, and cellulose. Further, with such a resin, it is possible to easily form a hollow fiber membrane that selectively permeates water.
【００１１】ポッテイング剤（２）、（３）としては、
エポキシ樹脂、シリコン樹脂、ポリウレタン樹脂などが
例示できる。ポッテイング剤（２）、（３）の中、少な
くとも、中空糸膜（１）の開口端（４）側に位置するポ
ッテイング剤（２）の被覆厚さ（ｔ）は、中空糸膜
（１）の束の直径（ａ）に対して２〜３０％、好ましく
は３〜１５％の範囲とするのが望ましい。ここに、中空
糸膜（１）の束の直径（ａ）とは、中空糸膜（１）の断
面が円形でない場合においては、断面における最長の直
線、例えば、断面が楕円の場合は長径を意味する。そし
て、ポッテイング剤（２）の被覆厚さ（ｔ）は、その厚
さが一定でない場合においては、最も薄い厚さを意味す
る。従って、ポッテイング剤（２）の被覆厚さ（ｔ）が
一定でない場合、中空糸膜（１）の束の直径（ａ）に対
する被覆厚さ（ｔ）は、最も薄い箇所の厚さが２％以上
であり、最も厚い箇所の厚さが３０％以下となっていれ
ばよい。As the potting agents (2) and (3),
Examples thereof include epoxy resin, silicone resin, polyurethane resin and the like. Among the potting agents (2) and (3), at least the coating thickness (t) of the potting agent (2) located on the open end (4) side of the hollow fiber membrane (1) is the hollow fiber membrane (1). It is desirable that the range is 2 to 30%, preferably 3 to 15% with respect to the diameter (a) of the bundle. Here, the diameter (a) of the bundle of hollow fiber membranes (1) means the longest straight line in the cross section when the cross section of the hollow fiber membrane (1) is not circular, for example, the major axis when the cross section is elliptical. means. The coating thickness (t) of the potting agent (2) means the thinnest thickness when the thickness is not constant. Therefore, when the coating thickness (t) of the potting agent (2) is not constant, the coating thickness (t) with respect to the diameter (a) of the bundle of hollow fiber membranes (1) is 2% at the thinnest portion. The above is sufficient, and the thickness of the thickest part may be 30% or less.
【００１２】中空糸膜（１）の束の直径（ａ）に対して
上記の被覆厚さ（ｔ）を２％以上とすることにより、ポ
ッテイング剤（２）のひび割れを一層効果的に防止でき
るが、３０％を超える場合は、膜面積に対するモジュー
ルの比率が大きくなり過ぎて空間効率が悪くなる。一
方、中空糸膜（１）の封止端（５）側に位置するポッテ
イング剤（３）の被覆厚さは、特に限定されず、ポッテ
イング剤（２）の被覆厚さと同じ厚さでもよく、また
は、これよりも薄くてもよい。When the coating thickness (t) is 2% or more with respect to the diameter (a) of the bundle of hollow fiber membranes (1), cracking of the potting agent (2) can be more effectively prevented. However, if it exceeds 30%, the ratio of the module to the membrane area becomes too large, resulting in poor space efficiency. On the other hand, the coating thickness of the potting agent (3) located on the sealing end (5) side of the hollow fiber membrane (1) is not particularly limited, and may be the same as the coating thickness of the potting agent (2), Alternatively, it may be thinner than this.
【００１３】本発明において、中空糸膜モジュールは、
従来公知の方法に従い、図３に示すように、ハウジング
（９）内に収納されて用いられる。本発明で用いられる
ハウジング（９）においては、一方の側面が閉止され、
他方の側面に透過蒸気抜き出し口（８）が設けられ、中
間部の２箇所には、閉止側面に近い方から順次原料供給
口（６）と非透過液抜き出し口（７）が備えられてい
る。そして、中空糸膜モジュールは、中空糸膜（１）の
開口端（４）側がハウジング（９）の透過蒸気抜き出し
口（８）に位置するように収納され、Ｏリング（１０）
により開口端（４）側でシールされる。In the present invention, the hollow fiber membrane module is
According to a conventionally known method, as shown in FIG. 3, it is housed in a housing (9) for use. The housing (9) used in the present invention has one side closed,
A permeated vapor extraction port (8) is provided on the other side face, and a raw material supply port (6) and a non-permeated liquid extraction port (7) are sequentially provided at two positions in the middle part from the side closer to the closed side face. . The hollow fiber membrane module is housed so that the open end (4) side of the hollow fiber membrane (1) is located at the permeated vapor extraction port (8) of the housing (9), and the O-ring (10).
To seal on the open end (4) side.
【００１４】そして、中空糸膜（１）の２次側（中空糸
膜の内側）は、透過蒸気抜き出し口（８）側に接続され
た真空ポンプ（図示せず）により減圧にされる。中空糸
膜（１）の２次側（中空糸膜の内側）の減圧度は、通
常、１〜２００トール、好ましくは、３〜３０トールの
範囲から適宜選択される。分離対象液は、原料供給口
（６）から中空糸膜（１）の１次側（中空糸膜の外側）
に供給され、非透過成分は、中空糸膜（１）の外側を流
れて非透過液抜き出し口（７）から抜き出される。気化
して中空糸膜（１）を透過した透過成分（蒸気）は、透
過蒸気抜き出し口（８）から抜き出され、凝縮器（図示
せず）で液化される。The secondary side of the hollow fiber membrane (1) (the inside of the hollow fiber membrane) is decompressed by a vacuum pump (not shown) connected to the permeated vapor extraction port (8) side. The degree of pressure reduction on the secondary side of the hollow fiber membrane (1) (inside the hollow fiber membrane) is usually 1 to 200 Torr, and preferably 3 to 30 Torr. The liquid to be separated is from the raw material supply port (6) to the primary side of the hollow fiber membrane (1) (outside the hollow fiber membrane).
The non-permeable component is supplied to the hollow fiber membrane (1) and flows out of the hollow fiber membrane (1) to be extracted from the non-permeable liquid extraction port (7). The permeation component (vapor) that has been vaporized and permeated through the hollow fiber membrane (1) is extracted from the permeation vapor extraction port (8) and liquefied by a condenser (not shown).
【００１５】上記のように構成された分離装置において
は、分離対象液が供給される１次側が中空糸膜（１）の
外側となり、気体が透過する２次側が中空糸膜（１）の
内側となる。従って、中空糸膜（１）の内側は、常に乾
燥されているため、中空糸膜（１）の膨潤は起こり難
い。しかも、例えば、分離対象液が水溶性有機溶剤と水
との混合液体であり、中空糸膜モジュールが水を選択的
に透過させる中空糸膜の場合においては、中空糸膜
（１）の２次側（中空糸膜の内側）を流れる蒸気の組成
は、水が濃縮された組成となる。In the separation device constructed as described above, the primary side to which the liquid to be separated is supplied is the outside of the hollow fiber membrane (1), and the secondary side through which the gas permeates is the inside of the hollow fiber membrane (1). Becomes Therefore, since the inside of the hollow fiber membrane (1) is always dried, swelling of the hollow fiber membrane (1) hardly occurs. Moreover, for example, in the case where the liquid to be separated is a mixed liquid of a water-soluble organic solvent and water, and the hollow fiber membrane module is a hollow fiber membrane that selectively permeates water, the secondary fiber of the hollow fiber membrane (1) is used. The composition of the steam flowing on the side (inside the hollow fiber membrane) is a composition in which water is concentrated.
【００１６】そして、好ましい態様に従い、中空糸膜
（１）の開口端（４）側に位置するポッテイング剤
（２）の被覆厚さ（ｔ）を中空糸膜（１）の束の直径
（ａ）に対して２〜３０％の範囲にした場合は、ポッテ
イング剤（２）のひび割れの可能性を一層小さくするこ
とが出来る。しかも、本発明においては、中空糸膜
（１）の外側から内側へ圧力が付与されるため、中空糸
膜（１）の内側から外側へ圧力が付与される従来の分離
方法に比し、圧力バランス的観点からしてもポッテイン
グ剤のひび割れを誘引する可能性が小さい。Then, according to a preferred embodiment, the coating thickness (t) of the potting agent (2) located on the open end (4) side of the hollow fiber membrane (1) is set to the diameter (a) of the bundle of hollow fiber membranes (1). 2) to 30%, the possibility of cracking of the potting agent (2) can be further reduced. Moreover, in the present invention, since pressure is applied from the outside to the inside of the hollow fiber membrane (1), the pressure is higher than that in the conventional separation method in which the pressure is applied from the inside to the outside of the hollow fiber membrane (1). Even from a balance point of view, there is little possibility of inducing cracks in the potting agent.
【００１７】[0017]
【実施例】以下、本発明を実施例により更に詳細に説明
するが、本発明は、その要旨を超えない限り、実施例に
より何ら限定されるものではない。 実施例１ 図１及び２に示す一端のみが開放端に成された中空糸膜
モジュールを図３に示すようにハウジング内に収納して
構成した分離装置を用いた。中空糸膜モジュールとして
は、中空糸膜（１）がイソプロピルアルコール中で長手
方向に２％伸びるポリイミドで形成され、中空糸膜
（１）の束の直径（ａ）が約５０ｍｍ、中空糸膜（１）
の開放端側に位置するポッテイング剤（エポキシ樹脂）
の被覆厚さ（ｔ）が約３ｍｍである中空糸膜モジュール
を用いた。EXAMPLES The present invention will be described in more detail with reference to examples below, but the present invention is not limited to the examples as long as the gist thereof is not exceeded. Example 1 A separating device was used in which the hollow fiber membrane module shown in FIGS. 1 and 2 and having only one open end was housed in a housing as shown in FIG. In the hollow fiber membrane module, the hollow fiber membrane (1) is formed of polyimide that extends 2% in the longitudinal direction in isopropyl alcohol, and the diameter (a) of the bundle of hollow fiber membranes (1) is about 50 mm. 1)
Potting agent (epoxy resin) located on the open end side of
A hollow fiber membrane module having a coating thickness (t) of about 3 mm was used.
【００１８】分離対象液としてイソプロピルアルコール
−水混合液（イソプロピルアルコール８５重量％）を用
い、図３に示す分離装置において、透過蒸気抜き出し口
（８）側に接続された真空ポンプ（図示せず）により、
２次側（中空糸膜の内側）を７トールの減圧状態とし、
原料供給口（６）から分離対象液を供給した。非透過液
抜き出し口（７）からイソプロピルアルコール−が濃縮
された混合液を抜き出し、透過蒸気抜き出し口（８）か
ら水が濃縮された組成の蒸気を抜き出して凝縮器（図示
せず）で液化した。液温８０℃で１００時間の連続運転
の結果、ポッテイング剤のひび割れは発生しなかった。A vacuum pump (not shown) connected to the permeated vapor extraction port (8) side in the separation apparatus shown in FIG. 3 using an isopropyl alcohol-water mixed liquid (85% by weight of isopropyl alcohol) as a liquid to be separated. Due to
The secondary side (the inside of the hollow fiber membrane) is set to a reduced pressure state of 7 Torr,
The liquid to be separated was supplied from the raw material supply port (6). The non-permeated liquid outlet (7) was used to withdraw the isopropyl alcohol-enriched mixed liquid, the permeated vapor outlet (8) was used to withdraw water-concentrated vapor, and the liquid was liquefied by a condenser (not shown). . As a result of continuous operation at a liquid temperature of 80 ° C. for 100 hours, cracking of the potting agent did not occur.
【００１９】実施例２ 実施例１において、中空糸膜（１）の開放端側に位置す
るポッテイング剤（エポキシ樹脂）の被覆厚さ（ｔ）の
みを約０．５ｍｍに変更した中空糸膜モジュールを用い
た以外は、実施例１と同様にしてイソプロピルアルコー
ル−水混合液の分離を行った。連続運転の結果、約６０
時間後にポッテイング剤のひび割れが生じた。Example 2 In Example 1, the hollow fiber membrane module was modified such that only the coating thickness (t) of the potting agent (epoxy resin) located on the open end side of the hollow fiber membrane (1) was changed to about 0.5 mm. Isopropyl alcohol-water mixture was separated in the same manner as in Example 1 except that was used. About 60 as a result of continuous operation
After the time, the potting agent cracked.
【００２０】比較例１ ハウジング内に両端開放型モジュールを収納した図４に
示す従来の分離装置を用いた。中空糸膜モジュールとし
ては、中空糸膜（１）がイソプロピルアルコール中で長
手方向に２％伸びるポリイミドで形成され、中空糸膜
（１）の束の直径（ａ）が約５０ｍｍ、ポッテイング剤
（エポキシ樹脂）の被覆厚さ（ｔ）が約１ｍｍである中
空糸膜モジュールを用いた。実施例１と同様の分離対象
液を用い、透過蒸気抜き出し口（８）側に接続された真
空ポンプ（図示せず）により、２次側（中空糸膜の内
側）を７トールの減圧状態とし、原料供給口（６）から
分離対象液を供給した。非透過液抜き出し口（７）から
イソプロピルアルコール−が濃縮された混合液を抜き出
し、透過蒸気抜き出し口（８）から水が濃縮された組成
の蒸気を抜き出して凝縮器（図示せず）で液化した。液
温８０℃で連続運転を行った結果、約２５時間後にポッ
テイング剤のひび割れが生じた。Comparative Example 1 A conventional separating device shown in FIG. 4 in which a module having open-ended ends is housed in a housing was used. As the hollow fiber membrane module, the hollow fiber membrane (1) is formed of polyimide that extends 2% in the longitudinal direction in isopropyl alcohol, the diameter (a) of the bundle of hollow fiber membranes (1) is about 50 mm, and the potting agent (epoxy) is used. A hollow fiber membrane module having a coating thickness (t) of resin) of about 1 mm was used. Using the same liquid to be separated as in Example 1, the secondary side (inside the hollow fiber membrane) was depressurized to 7 Torr by a vacuum pump (not shown) connected to the permeation vapor extraction port (8) side. The liquid to be separated was supplied from the raw material supply port (6). The non-permeated liquid outlet (7) was used to withdraw the isopropyl alcohol-enriched mixed liquid, the permeated vapor outlet (8) was used to withdraw water-concentrated vapor, and the liquid was liquefied by a condenser (not shown). . As a result of continuous operation at a liquid temperature of 80 ° C., the potting agent cracked after about 25 hours.
【００２１】[0021]
【発明の効果】以上説明した本発明によれば、中空糸膜
モジュールを構成するポッテイング剤のひび割れを防止
し、長時間の連続運転を行う得るように改良された浸透
気化による分離方法が提供され、本発明の工業的価値は
顕著である。According to the present invention described above, there is provided a separation method by pervaporation which is improved so as to prevent the potting agent constituting the hollow fiber membrane module from cracking and to carry out continuous operation for a long time. The industrial value of the present invention is remarkable.
【図１】本発明の分離方法に用いられる中空糸膜モジュ
ールの一例の模式的断面説明図である。FIG. 1 is a schematic cross-sectional explanatory view of an example of a hollow fiber membrane module used in the separation method of the present invention.
【図２】図１のＡ−Ａ線の断面図である。FIG. 2 is a cross-sectional view taken along the line AA of FIG.
【図３】本発明の分離方法を示す説明図である。FIG. 3 is an explanatory diagram showing a separation method of the present invention.
【図４】従来の分離方法の説明図である。FIG. 4 is an explanatory diagram of a conventional separation method.
１：中空糸 ２：ポッテイング材 ３：ポッテイング材 ４：開口端 ５：封止端 ６：原料供給口 ７：非透過液抜き出し口 ８：透過蒸気抜き出し口 ９：ハウジング 10：Ｏリング ｔ：ポッテイング材の被覆厚さ ａ：中空糸膜の束の直径 1: Hollow fiber 2: Potting material 3: Potting material 4: Opening end 5: Sealing end 6: Raw material supply port 7: Non-permeate extraction port 8: Permeation vapor extraction port 9: Housing 10: O-ring t: Potting material Coating thickness a: Diameter of bundle of hollow fiber membranes
Claims (3)
よる分離方法において、中空糸膜モジュールとして、多
数の中空糸膜（１）が束状に引き揃えられ、その両端が
ポッテイング剤（２）、（３）で相互に固定され、一端
側の各中空糸膜（１）の先端がポッテイング剤の端面に
露出して開口端（４）を形成し、他端側の各中空糸膜
（１）の先端がポッテイング剤中に埋没されて封止端
（５）を形成して成る中空糸膜モジュールを用い、そし
て、中空糸膜（１）の内側を減圧状態とすることによ
り、中空糸膜（１）の外側から内側に透過成分を移動さ
せることを特徴とする分離方法。1. A method for separating by pervaporation using a hollow fiber membrane module, wherein as a hollow fiber membrane module, a large number of hollow fiber membranes (1) are aligned in a bundle, and both ends thereof are potting agents (2). The hollow fiber membranes (1) are fixed to each other at (3), the tips of the hollow fiber membranes (1) on one end side are exposed at the end face of the potting agent to form open ends (4), and the hollow fiber membranes (1) on the other end side are formed. By using a hollow fiber membrane module in which the tip of the hollow fiber membrane is embedded in a potting agent to form a sealed end (5), and the inside of the hollow fiber membrane (1) is depressurized, the hollow fiber membrane ( 1) A separation method characterized by moving a permeation component from the outside to the inside.
手軸方向に０．５％以上伸びる素材で形成されている請
求項１に記載の分離方法。2. The separation method according to claim 1, wherein the hollow fiber membrane is formed of a material that extends 0.5% or more in the longitudinal axis direction when immersed in the liquid to be separated.
するポッテイング剤の被覆厚さが中空糸膜の束の直径に
対して２〜３０％の範囲である請求項１又は２に記載の
分離方法。3. The coating thickness of the potting agent located at the open end side of the hollow fiber membrane is at least in the range of 2 to 30% with respect to the diameter of the bundle of hollow fiber membranes. Separation method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7123993A JPH06254355A (en) | 1993-03-05 | 1993-03-05 | Separation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7123993A JPH06254355A (en) | 1993-03-05 | 1993-03-05 | Separation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06254355A true JPH06254355A (en) | 1994-09-13 |
Family
ID=13454954
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7123993A Withdrawn JPH06254355A (en) | 1993-03-05 | 1993-03-05 | Separation |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06254355A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020111158A1 (en) * | 2018-11-27 | 2020-06-04 | 旭化成株式会社 | Membrane distillation module and membrane distillation apparatus |
-
1993
- 1993-03-05 JP JP7123993A patent/JPH06254355A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020111158A1 (en) * | 2018-11-27 | 2020-06-04 | 旭化成株式会社 | Membrane distillation module and membrane distillation apparatus |
| US12194416B2 (en) | 2018-11-27 | 2025-01-14 | Asahi Kasei Kabushiki Kaisha | Membrane distillation module and membrane distillation apparatus |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2872521B2 (en) | Two-stage membrane separation drying method and apparatus | |
| US4180388A (en) | Processes | |
| US5013437A (en) | Hollow fiber membrane fluid separation device adapted for boreside feed which contains multiple concentric stages | |
| EP0702995B1 (en) | Membrane gas separation | |
| US6224763B1 (en) | Hollow-fiber membrane device including a split disk tube sheet support | |
| US6565631B2 (en) | High carbon content filamentary membrane and method of making the same | |
| US5158581A (en) | Fluid separation membrane module with hollow fibers having segregated active surface regions | |
| KR940004619B1 (en) | Gas Separation Method Using Spirally Wound Perforated Fiber Cartridge Cartridge | |
| AU2003247716B2 (en) | Processes and apparatus using solid perm-selective membranes in multiple groups for simultaneous recovery of specified products from a fluid mixture | |
| EP0540877A2 (en) | Double ended hollow fiber bundle and fluids separation apparatus | |
| JPH04265111A (en) | Method and device for drying using diaphragm | |
| JP2000262838A (en) | Gas separation membrane module and gas separation method | |
| JPH035309A (en) | Improved method and apparatus for producing dry high-purity nitrogen | |
| CA2351272A1 (en) | Membrane-assisted fluid separation apparatus and method | |
| EP1608446A1 (en) | Purification of fluid compounds utilizing a distillation-membrane separation process | |
| US4874405A (en) | Coupling fluid separation membrane elements | |
| JPH06254355A (en) | Separation | |
| JP2016041419A (en) | Separation method and separation apparatus | |
| JPH04176303A (en) | Method for removing gas dissolved in liquid | |
| Strathman et al. | Development of synthetic membranes for gas and vapor separation | |
| JP3727552B2 (en) | Perfluoro compound gas separation and recovery equipment | |
| JP2002035530A (en) | Operation method of gas separation membrane | |
| JP2003159517A (en) | Hollow fiber separation membrane module | |
| Feng et al. | Permeate pressure build‐up in shellside‐fed hollow fiber pervaporation membranes | |
| JP2023063385A (en) | Separation membrane module |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 20000509 |