JP3262855B2 - Hollow fiber membrane defect detection method - Google Patents
Hollow fiber membrane defect detection methodInfo
- Publication number
- JP3262855B2 JP3262855B2 JP25266492A JP25266492A JP3262855B2 JP 3262855 B2 JP3262855 B2 JP 3262855B2 JP 25266492 A JP25266492 A JP 25266492A JP 25266492 A JP25266492 A JP 25266492A JP 3262855 B2 JP3262855 B2 JP 3262855B2
- Authority
- JP
- Japan
- Prior art keywords
- hollow fiber
- fiber membrane
- detecting
- defect
- film
- 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 - Fee Related
Links
Landscapes
- Length Measuring Devices By Optical Means (AREA)
- Investigating Materials By The Use Of Optical Means Adapted For Particular Applications (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、中空糸膜分離装置に用
いる中空糸膜の欠陥を検出する方法に関する。The present invention relates to a method for detecting a defect in a hollow fiber membrane used in a hollow fiber membrane separation device.
【０００２】[0002]
【従来の技術】中空糸膜分離装置（中空糸膜モジュー
ル）には一般に数百から数万の中空糸膜が充填されてお
りそのうちの一本でも膜壁に貫通部のような欠陥があっ
た場合は、未処理流体と処理済流体が混ざってしまい実
用にならない。そこで、こうした欠陥を検出するために
いくつかの工夫がなされ、特開昭５５−７０２５８号公
報、特開昭５６−１２０９９３号公報、特開昭５６−１
２９００３号公報、特開昭５６−１２９００４号公報、
特開昭６０−９４１０５号公報、特公昭５６−３９９２
１号公報、特公昭５７−１８９２３号公報等に技術が開
示されている。このうち、特開昭５５−７０２５８号公
報にはモジュールの端部に水等を張り、中空糸膜外から
気圧をかけ、欠陥中空糸膜のみ欠陥部から注入された気
体が液内で気柱を形成するのを目視する方法が開示され
ている。しかし、以上の方法は、中空糸膜モジュールに
なってから検出する方法であり、モジュール化の時点で
生じる欠陥の検出もできるが、中空糸膜に存在する欠陥
はモジュール化の前に検出すれば、モジュール化の手間
とコストと時間を省くことができる。2. Description of the Related Art Generally, a hollow fiber membrane separation device (hollow fiber membrane module) is filled with hundreds to tens of thousands of hollow fiber membranes, and even one of them has a defect such as a penetration portion in the membrane wall. In such a case, the unprocessed fluid and the processed fluid are mixed, which is not practical. In order to detect such a defect, some measures have been taken, and Japanese Patent Application Laid-Open Nos. 55-70258, 56-120993, and 56-1 are disclosed.
No. 29003, JP-A-56-129004,
JP-A-60-94105, JP-B-56-3992
No. 1, JP-B-57-18923, and the like disclose the technology. Among them, Japanese Patent Application Laid-Open No. 55-70258 discloses that water or the like is applied to the end of a module, pressure is applied from the outside of the hollow fiber membrane, and only the defective hollow fiber membrane has a gas injected in the liquid through the air column. Are disclosed. However, the above method is a method of detecting a hollow fiber membrane module and then detecting the defect.Although a defect generated at the time of modularization can be detected, a defect existing in the hollow fiber membrane can be detected before modularization. In addition, the labor, cost and time for modularization can be saved.
【０００３】そこで、中空糸膜の状態で検出する方法の
例としては、特開昭５６−２２９２２号公報に開示され
ているように中空糸膜の中空部に液体を充填後加圧気体
と接触させ、欠陥から注入された気泡の存在を静電容量
変化から検出する方法がある。Therefore, as an example of a method of detecting the state of the hollow fiber membrane, as disclosed in JP-A-56-22922, the hollow part of the hollow fiber membrane is filled with a liquid and then contacted with a pressurized gas. Then, there is a method of detecting the presence of bubbles injected from a defect from a change in capacitance.
【０００４】[0004]
【発明が解決しようとする課題】しかしこの方法は欠陥
部に気体を押し込むための前処理が必要であり、また膜
に傷をつける危険性がある。本発明者は、こうした前処
理が不要であり、かつ膜に非接触で中空糸膜の異物由来
の膜壁欠陥部の存在を検出する方法を探索し本発明に到
達した。However, this method requires a pretreatment for forcing gas into the defective portion, and there is a risk of damaging the film. The present inventor has found that such pretreatment is unnecessary, and the non-contact with the membrane is caused by the foreign matter of the hollow fiber membrane.
The present inventors have searched for a method for detecting the presence of a film wall defect, and have arrived at the present invention.
【０００５】[0005]
【課題を解決するための手段】すなわち本発明は、
（１）中空糸膜製膜において、空中走行部の製膜中の中
空糸膜の外径を測定し、その変化を検知することを特徴
とする中空糸膜欠陥検出方法である。（２）変化を検知
し、異物由来の膜壁欠陥部の存在を検出することを特徴
とする（１）記載の中空糸膜欠陥検出方法である。
（３）中空糸膜製膜がポリマー溶液を円環状紡口から内
部凝固液とともに吐出し凝固浴中にて凝固させる方法で
あることを特徴とする（２）記載の中空糸膜欠陥検出方
法である。（４）空中走行部がポリマー溶液を紡口から
吐出してから凝固浴に入るまでの間にあることを特徴と
する（３）記載の中空糸膜欠陥検出方法である。（５）
測定が、中空糸膜の走行方向に対し互いに直行するＸ方
向Ｙ方向からの２方向からの測定である事を特徴とする
請求項１乃至４記載の中空糸膜検出方法である。まず、
本発明の原理を説明する。中空糸膜の形成は、ポリマー
溶液を円環状紡口から吐出し直接あるいは空気中を走行
後凝固浴中にて凝固させておこなわせしめる。このポリ
マー溶液中に異物があった場合、中空糸膜の欠陥として
現れる。異物が固形物の場合、膜内外表面にはみ出した
り、それが原因で凝固が一様でなくなり、凹凸ができ膜
破れしやすくなる場合がある。異物が気泡の場合、気泡
が膜厚に対して小さければ膜中に潜在欠陥として残留す
るが、ある程度大きいと製膜時、空中走行部を走行中に
内部凝固液の圧力で膜壁が破れ顕在欠陥となる。この
時、内部凝固液が空中に飛び出し、また、飛び出した内
部凝固液が膜外壁を流れ落ちて外表面に凹凸を作ったり
くびれたりする。このように中空糸膜の顕在欠陥の多く
は外径異常として現れることが多い。本発明者はこの外
径異常に着目し、製膜中の中空糸膜の外径変化を観測し
ていて異常を検出したときには、多くは、問題にしてい
る製膜欠陥が検出できることを見いだした。That is, the present invention provides:
(1) In a hollow fiber membrane film formation, within in film of aeration feeding region
A hollow fiber membrane defect detection method characterized by measuring the outer diameter of a hollow fiber membrane and detecting a change . (2) Detect changes
And detects the presence of film wall defects due to foreign matter.
(1) The hollow fiber membrane defect detection method according to (1).
(3) Hollow fiber membrane formation allows polymer solution to enter from annular spout
With coagulation liquid and coagulation in coagulation bath
The method for detecting a hollow fiber membrane defect according to (2), wherein
Is the law. (4) The aerial traveling section starts the polymer solution from the spout
It is characterized by being between discharge and before entering the coagulation bath
(3) The hollow fiber membrane defect detection method according to (3). (5)
Measurement is performed in the X direction perpendicular to the running direction of the hollow fiber membrane.
The measurement is performed from two directions from the Y direction.
A method for detecting a hollow fiber membrane according to any one of claims 1 to 4. First,
The principle of the present invention will be described. The hollow fiber membrane is formed by discharging a polymer solution from an annular spinneret or by coagulating in a coagulation bath directly or after running in air. If there is a foreign substance in the polymer solution, it appears as a defect in the hollow fiber membrane. When the foreign matter is a solid, it may protrude into the inner and outer surfaces of the film, and due to this, the solidification may not be uniform, and irregularities may be formed to easily break the film. If the foreign matter is a bubble, if the bubble is smaller than the film thickness, it will remain as a latent defect in the film, but if it is somewhat large, the film wall will be broken by the pressure of the internal coagulation liquid during running in the air running part during film formation. It becomes a defect. At this time, the internal coagulating liquid jumps out into the air, and the protruding internal coagulating liquid flows down the outer wall of the membrane to form irregularities or constrictions on the outer surface. As described above, most of the obvious defects of the hollow fiber membrane often appear as outer diameter abnormalities. The present inventors have paid attention to this outer diameter abnormality, and when observing the change in the outer diameter of the hollow fiber membrane during film formation and detecting the abnormality, it has been found that in many cases, the film forming defect in question can be detected. .
【０００６】そして、鋭意研究の結果、凝固浴等を出た
後でも検出可能であるが凝固浴の媒体が付着するため付
着液体を拭き取らないと外径変化が正確にとらえられな
いことがあり膜に傷を付けるおそれがあること、従って
紡口吐出後の空中走行部での検出の方が好ましいこと、
検出の方法は、レーザーを走査させて外径を算出する方
法、ビデオカメラで観測し画像処理する方法等が考えら
れるがレーザーを用いたセンサが簡便、正確、迅速で好
ましいことなどがわかった。[0006] As a result of intensive studies, it is possible to detect even after leaving the coagulation bath, etc., but since the medium in the coagulation bath adheres, the change in outer diameter cannot be accurately detected unless the adhered liquid is wiped off. That there is a risk of damaging the film, and that detection in the aerial traveling section after the spout ejection is more preferable,
As a detection method, a method of calculating an outer diameter by scanning a laser, a method of performing image processing by observing with a video camera, and the like can be considered, and it has been found that a sensor using a laser is simple, accurate, rapid, and preferable.
【０００７】[0007]
【実施例】本発明の欠陥検出方法を用いた製膜装置を実
施例を用いて具体的に説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A film forming apparatus using the defect detection method of the present invention will be specifically described with reference to embodiments.
【０００８】[0008]
【実施例１】図１は、本発明の中空糸膜製膜装置の例の
概略図である。ポリマー溶液はタンク（１）から定量ギ
アポンプ（２）を通じて円環状紡口（３）から吐出さ
れ、空中を走行し凝固浴（５）に導入され凝固する。こ
こで空中走行部に外径検出機（４）を設置する。実施例
１ではレーザー外径検出機を設置した。この検出機の出
力信号はチャート等に記録管理される一方、そこである
異常を検出したら、巻き取り装置のトラバース装置
（６）が移動して、検出された欠陥のある部分の中空糸
膜は枠（７）に取り付けてある予備枠（８）に巻き付け
られ製品となる束からは外され、正常部になると元の枠
（７）に巻き付けられるようにシーケンスが組まれてい
る。巻き取り装置部は、定長切断装置でも良い。その場
合は欠陥部を含む部分が定長切断された後系外へはじき
出される。Embodiment 1 FIG. 1 is a schematic view of an example of a hollow fiber membrane forming apparatus of the present invention. The polymer solution is discharged from the annular spinneret (3) through the metering gear pump (2) from the tank (1), travels in the air, is introduced into the coagulation bath (5), and solidifies. Here, an outer diameter detector (4) is installed in the aerial traveling section. In Example 1, a laser outer diameter detector was installed. While the output signal of this detector is recorded and managed in a chart or the like, if an abnormality is detected there, the traverse device (6) of the winding device moves and the hollow fiber membrane of the detected defective portion is framed. The sequence is set so that the spare frame (8) attached to (7) is wound around the original frame (7) when it is wound out of the bundle that is to be a product by being wound around the spare frame (8). The winding device may be a fixed length cutting device. In that case, the portion including the defective portion is cut out to a fixed length and then ejected out of the system.
【０００９】[0009]
【実施例２】図１に示した製膜装置の空中走行部にレー
ザー外径測定機（（株）キーエンス製、測定部はＬＳ−
３０３６、コントローラー部はＬＳ−３００２）を設置
した。ポリスルホン２０重量部、Ｎ−メチル−２−ピロ
リドン８０重量部の均一溶解ポリマー溶液を１気圧に加
圧しながらタンク（１）定量ギアポンプ（２）に送り、
１分間に１２ｃｃずつ吐出させた。紡口（３）の各部の
寸法は、図２においてａ＝０．６ｍｍ、ｂ＝０．９ｍ
ｍ、ｃ＝１．８ｍｍ、ポリマー溶液温度は２０℃、空中
走行距離は６ｃｍ、凝固浴温度は３０℃、巻き取り速度
は毎分１１ｍであった。Embodiment 2 A laser outer diameter measuring machine (manufactured by KEYENCE CORPORATION, measuring unit: LS-
3036, the controller section was provided with LS-3002). A homogeneously dissolved polymer solution of 20 parts by weight of polysulfone and 80 parts by weight of N-methyl-2-pyrrolidone is sent to a tank (1) fixed-quantity gear pump (2) while pressurizing to 1 atm.
The liquid was discharged at a rate of 12 cc per minute. The dimensions of each part of the spout (3) are a = 0.6 mm and b = 0.9 m in FIG.
m, c = 1.8 mm, the polymer solution temperature was 20 ° C., the air travel distance was 6 cm, the coagulation bath temperature was 30 ° C., and the winding speed was 11 m / min.
【００１０】図３に外径検出機（４）からの出力を示
す。ギアポンプの吐出むらのため外径変動が検出されて
いる。紡糸開始後５分、ポリマー溶液中に気泡があった
らしく内部凝固液が飛び出したのが目撃された。この時
外径検出機のチャート上にピークが現れ、異常検出警報
と共に巻き取り枠のトラバース装置（６）が異常側へ動
き、製品枠（７）の外の予備枠（８）に巻き取りを変更
した。予備枠の中空糸膜を見てみると、このピークに対
応する部分の中空糸膜が巻き取られており、観察する
と、図４のスケッチのように膜壁に穴があいておりくび
れていた。図３中のピークＣは内部凝固液の飛び出し、
ピークＤはくびれに相当するものと推定される。FIG. 3 shows the output from the outer diameter detector (4). Outer diameter fluctuation is detected due to uneven discharge of the gear pump. Five minutes after the start of spinning, it was observed that air bubbles appeared in the polymer solution and the internal coagulation liquid jumped out. At this time, a peak appears on the chart of the outer diameter detector, and together with the abnormality detection alarm, the traverse device (6) of the winding frame moves to the abnormal side, and the winding is performed on the spare frame (8) outside the product frame (7). changed. Looking at the hollow fiber membrane of the preliminary frame, the hollow fiber membrane corresponding to this peak was wound up, and when observed, it had a hole in the membrane wall as shown in the sketch in FIG. . The peak C in FIG.
Peak D is presumed to correspond to constriction.
【００１１】[0011]
【発明の効果】以上述べたように、本発明の方法、装置
により、外径変化に現れる中空糸膜の異物由来の膜壁欠
陥部の存在を非接触で、かつ何の前処理もなしに検出す
る事が可能である。さらに、本発明では、ギアポンプの
吐出異常等による外径変動もとらえられる。As described above, according to the method and apparatus of the present invention, the presence of the membrane wall defect due to the foreign matter of the hollow fiber membrane appearing in the change of the outer diameter can be determined in a non-contact manner. It is possible to detect without pre-processing. Further, in the present invention, the outer diameter fluctuation due to the abnormal discharge of the gear pump or the like can be detected.
【００１２】また、中空糸膜断面が真円状でなく、楕円
状であると膜厚むらがあると薄いところが使用中に破れ
たりする危険があるが、こうした異常もＸ方向Ｙ方向２
基の検出機を装備することで検出できる。こうした効果
は従来技術の欠陥検出装置には期待できないものであ
る。If the cross section of the hollow fiber membrane is not a perfect circle but an ellipse, there is a danger that a thin portion may be broken during use if the film thickness is uneven.
It can be detected by equipping a base detector. Such an effect cannot be expected from the conventional defect detection apparatus.
【図１】本発明の中空糸膜製膜装置の例の概略図であ
る。（Ａ）は枠の側面図、（Ｂ）は枠の正面図である。FIG. 1 is a schematic view of an example of a hollow fiber membrane forming apparatus of the present invention. (A) is a side view of a frame, (B) is a front view of a frame.
【図２】環状紡口の拡大図である。FIG. 2 is an enlarged view of an annular spout.
【図３】外径検出機からの出力例を示す。FIG. 3 shows an output example from an outer diameter detector.
【図４】実施例２で得た製膜欠陥のスケッチである。FIG. 4 is a sketch of a film formation defect obtained in Example 2.
１ ポリマー溶液タンク ２ 定量ギアポンプ ３ 環状紡口 ４ 外径検出機 ５ 凝固浴 ６ トラバース装置 ７ 巻き取り枠 ８ 予備枠 ９ 内部凝固液タンク １０ 内部凝固液定量ポンプ REFERENCE SIGNS LIST 1 polymer solution tank 2 metering gear pump 3 annular spinner 4 outer diameter detector 5 coagulation bath 6 traverse device 7 winding frame 8 spare frame 9 internal coagulating liquid tank 10 internal coagulating liquid measuring pump
フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) B01D 65/10 B01D 69/08 G01B 11/10 G01N 21/89 Continuation of the front page (58) Field surveyed (Int.Cl. 7 , DB name) B01D 65/10 B01D 69/08 G01B 11/10 G01N 21/89
Claims (5)
膜中の中空糸膜の外径を測定し、その変化を検知するこ
とを特徴とする中空糸膜欠陥検出方法。1. A hollow fiber membrane made of film, manufacturing of aeration feeding region
A method for detecting a defect in a hollow fiber membrane , comprising measuring an outer diameter of the hollow fiber membrane in the membrane and detecting a change in the outer diameter.
存在を検出することを特徴とする請求項１記載の中空糸The hollow fiber according to claim 1, wherein the presence is detected.
膜欠陥検出方法。Film defect detection method.
口から内部凝固液とともに吐出し凝固浴中にて凝固させDischarge with internal coagulation liquid from mouth and coagulate in coagulation bath
る方法であることを特徴とする請求項２記載の中空糸膜3. The hollow fiber membrane according to claim 2, wherein
欠陥検出方法。Defect detection method.
出してから凝固浴に入るまでの間にあることを特徴とすIt is characterized by being between the time of taking out and entering the coagulation bath
る請求項３記載の中空糸膜欠陥検出方法。The method for detecting a defect in a hollow fiber membrane according to claim 3.
に直行するＸ方向Ｙ方向からの２方向からの測定であるIs a measurement from two directions from the X direction and the Y direction orthogonal to
事を特徴とする請求項１乃至４記載の中空糸膜検出方The method for detecting a hollow fiber membrane according to claim 1, wherein
法。Law.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25266492A JP3262855B2 (en) | 1992-09-22 | 1992-09-22 | Hollow fiber membrane defect detection method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25266492A JP3262855B2 (en) | 1992-09-22 | 1992-09-22 | Hollow fiber membrane defect detection method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0699043A JPH0699043A (en) | 1994-04-12 |
| JP3262855B2 true JP3262855B2 (en) | 2002-03-04 |
Family
ID=17240514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25266492A Expired - Fee Related JP3262855B2 (en) | 1992-09-22 | 1992-09-22 | Hollow fiber membrane defect detection method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3262855B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003535335A (en) * | 2000-05-31 | 2003-11-25 | ツエルヴエーゲル・ルーヴア・アクチエンゲゼルシヤフト | METHOD AND APPARATUS FOR CONFIRMING CONTAMINANTS IN FILT PRODUCTS LONGLY MOVED |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100302209B1 (en) * | 1999-04-27 | 2001-09-22 | 주덕영 | Manufacturing method of hdpe hollow fiber membrane by circulating drawing method and apparatus thereof |
| JP5094018B2 (en) * | 2005-12-28 | 2012-12-12 | 三菱レイヨン株式会社 | Method for producing hollow fiber membrane |
| CA2681056A1 (en) * | 2007-03-16 | 2008-10-23 | Asahi Kasei Chemicals Corporation | Method for inspecting defect of hollow fiber porous membrane, defect inspection equipment and production method |
| WO2013129004A1 (en) * | 2012-02-29 | 2013-09-06 | 東レ株式会社 | Manufacturing method and manufacturing device for bundle product |
-
1992
- 1992-09-22 JP JP25266492A patent/JP3262855B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003535335A (en) * | 2000-05-31 | 2003-11-25 | ツエルヴエーゲル・ルーヴア・アクチエンゲゼルシヤフト | METHOD AND APPARATUS FOR CONFIRMING CONTAMINANTS IN FILT PRODUCTS LONGLY MOVED |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0699043A (en) | 1994-04-12 |
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