JP2826823B2 - Manufacturing method of hollow fiber module - Google Patents
Manufacturing method of hollow fiber moduleInfo
- Publication number
- JP2826823B2 JP2826823B2 JP62260548A JP26054887A JP2826823B2 JP 2826823 B2 JP2826823 B2 JP 2826823B2 JP 62260548 A JP62260548 A JP 62260548A JP 26054887 A JP26054887 A JP 26054887A JP 2826823 B2 JP2826823 B2 JP 2826823B2
- Authority
- JP
- Japan
- Prior art keywords
- hollow fiber
- separation membrane
- type separation
- outer cylinder
- fiber type
- 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
- 239000012510 hollow fiber Substances 0.000 title claims description 47
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000012528 membrane Substances 0.000 claims description 38
- 238000000926 separation method Methods 0.000 claims description 33
- 238000004382 potting Methods 0.000 claims description 19
- 239000000853 adhesive Substances 0.000 claims description 11
- 230000001070 adhesive effect Effects 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 description 19
- 230000001954 sterilising effect Effects 0.000 description 8
- 238000004659 sterilization and disinfection Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 102000004190 Enzymes Human genes 0.000 description 4
- 108090000790 Enzymes Proteins 0.000 description 4
- 239000011942 biocatalyst Substances 0.000 description 4
- 229920002635 polyurethane Polymers 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/021—Manufacturing thereof
- B01D63/022—Encapsulating hollow fibres
- B01D63/0221—Encapsulating hollow fibres using a mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/021—Manufacturing thereof
- B01D63/022—Encapsulating hollow fibres
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、中空糸型分離膜を用いて種々の物質をろ過
する中空糸モジュールの製作方法に関し、更に詳しく
は、微生物等の生体触媒を利用して有用物質を生産する
手段として使用される中空糸モジュールの製作方法に関
する。
（従来の技術）
ふるいの原理によって種々の物質をろ過する能力を備
えた分離膜を使用した限外ろ過法が広く知られている。
第１図に示したものは、中空糸型分離膜を用いた中空
糸モジュールの一例で、多数本の中空糸型分離膜（１）
が流入口（３）及び流出口（３′）を付された外筒
（２）に挿入され、各中空糸型分離膜（１）及び外筒
（２）の両端部が接着剤によってポッティングされ、流
入孔（５）及び流出孔（５′）を付された蓋部材（４）
（４）が外筒（２）の両端部に被せられている。
中空糸型分離膜（１）は、孔径が数Å〜数μｍの範囲
のグレードが上市され、上記した中空糸モジュールは、
種々の用途に広く使用されており、中でも、近年におい
ては生体触媒を利用して有用物質を生産する、いわゆる
バイオリアクタへの応用に急速な成長を遂げている。
バイオリアクタにおける分離膜は、貴重な生体触媒を
バイオリアクタから濡らさぬ目的（固定化）と、生体触
媒が生産した有用物質を直接分離させて後工程の簡略化
を図る目的のために使用される。
バイオリアクタにおいては、他の雑菌の繁殖を防止す
るために、膜式又は回分式を問わず、運転開始前に滅菌
操作工程が実施され、この滅菌操作工程としては、通常
蒸気滅菌が行われ、120℃程度の高温蒸気中に10〜20分
間全ての接液部をさらすことによってなされる。
（発明が解決しようとする問題点）
上記した蒸気滅菌操作による熱衝撃を付与された中空
糸モジュールにおいては、構成部品の熱膨張率の違いに
よってもたらされる接着部の剥離現象及び中空糸型分離
膜の収縮に伴う中空糸型分離膜の欠損を生じることがあ
った。
すなわち、第１図に示すように、多数本の中空糸型分
離膜（１）及び外筒（２）の両端部を接着するポッティ
ング剤と外筒（２）との熱膨張率の違いにより、熱衝撃
を受けて接着面に剥離を生じ、そのためにリークを生じ
ることがあった。
この接着面の剥離現象は、ポッティング剤の硬さが、
ショアーＤ硬度で略85程度であって弾性が小さく、加熱
に伴って外筒及びポッティング剤間に発生する歪を吸収
し得ないために、接着部に付加される負担が大きくなる
ことによるものである。
次に、高分子系中空糸型分離膜は、高温にさらされた
際に、収縮を起す場合が多々ある。これは、相分離によ
ってもたらされる微細な網目構造が、高温における分子
間の熱運動により、更に安定した状態、つまり密な状態
になるためと考えられる。実際に、限外ろ過膜等を100
℃近い水蒸気雰囲気のもとに放置すると、透水量の減少
と分画曲線の低分子側への移動が起る。
そのために、第１図に示すように、両端部を接着剤で
ポッティングされた中空糸型分離膜（１）が、120℃の
水蒸気中にさらされて常温（20〜30℃）に戻された際に
おける収縮により、応力（張力）を付加されることにな
り、張力が或程度以上になると、膜の表面に微細なクラ
ックが発生し、その結果、菌体の漏出を惹起するおそれ
がある。
本発明は、上記した従来例の中空糸モジュールにおい
て、外筒に対する接着部におけるリークをもたらすポッ
テイング剤の剥離現象と、菌体の漏出を惹起させる中空
糸型分離膜の微細なクラックとを抑制し得る中空糸モジ
ュールの製作方法を提示することを目的するものであ
る。
（問題点を解決するための手段）
本発明は、上記した従来の製作方法による中空糸モジ
ュールにおける問題点を考慮して、外筒への挿入に先立
って、中空糸型分離膜を蒸気雰囲気中にさらして熱履歴
を付与し、その後中空糸型分離膜の多数本及び前記外筒
の端部をポッティング剤にて固定する構成となすもので
あり、さらにはそのポッティング剤がショアーＤ硬度略
50の接着剤である構成となすものである。
（作用）
上記した構成を備えた本発明による中空糸モジュール
の製作方法においては、熱履歴を付与された中空糸型分
離膜が、蒸気中での滅菌操作に伴う自らの収縮を抑制
し、さらには中空糸型分離膜及び外筒の端部のポッティ
ングに使用されたショアーＤ硬度略50でやや軟質の接着
剤が、蒸気中における滅菌によるポッティング部の剥離
現象を抑制する作用を示す。
（実施例）
ポリスルホン製中空糸型分離膜及びポリカーボネート
製モジュール外筒を用い、ポッティング剤として、日本
ポリウレタン社製Ｕ−537を主剤、ミリオネートMTL−Ｃ
を硬化剤とするポリウレタン（ポッティング剤）、又
は同社製Ｃ−11Aを主剤、Ｎ−148を硬化剤とするポリウ
レタン（ポッテイング剤）の組合せによって中空糸モ
ジュールを製作し、中空糸型分離膜に対し、外筒への接
着に先立って蒸気雰囲気中における加熱操作を付加した
もの及び付加しないものについて、蒸気滅菌操作後のリ
ークの有無を調査したところ、下記の結果が得られた。
ポッティング剤の硬さ： ショアーD84
ショアーD50
熱処理条件：オートクレーブ 120℃ １気圧
上記した試験結果から、中空糸型分離膜及び外筒の接
着工程に先立って中空糸分離膜に対し熱履歴を付与し、
更に、ポッティング剤として硬度の低い接着剤を使用す
るのが有効であることが立証された。
（発明の効果）
本発明による中空糸モジュールの製作方法が、上記し
たように、中空糸型分離膜をあらかじめ上記雰囲気中に
さらして、高温蒸気加熱で発生する膜の収縮等の熱履歴
を付与せしめてあるので、これら熱履歴を有する中空糸
型分離膜を組み込んで端部を固定した中空糸モジュール
は、その使用前にモジュール全体を高温蒸気の加熱操作
において、外筒の熱膨張と中空糸型分離膜の収縮とによ
り発生する分離膜への張力を少なくできるため、中空糸
型分離膜におけるクラック等の損傷の発生を格段に少な
く押さえられるというメリットが生ずる。
また、中空糸型分離膜および外筒とのポッティング剤
としてショアーＤ硬度略50と硬度が低く柔軟性を有する
接着剤を使用しているので高温蒸気処理時に発生する外
筒とポッティング剤との熱膨張の違いによる歪みを柔軟
に吸収できる。このため、外筒とポッティング剤間ある
いは中空糸とポッティング剤間の接着部剥離現象が有効
に抑えられる。
すなわち、中空糸型分離膜に蒸気加熱履歴を付与し、
さらに、ポッティング剤間をショアーＤ硬度略50の接着
剤とすることにより、製作完了後において蒸気雰囲気中
にさらされて滅菌操作を加えられても、中空糸型分離膜
の収縮に伴う亀裂及び接着部における剥離を生じること
がないので、従来の方法によって製作された中空糸モジ
ュールにおいて避けられなかった有用物質のリークのお
それが完全に解消する。Description: TECHNICAL FIELD The present invention relates to a method for producing a hollow fiber module for filtering various substances using a hollow fiber type separation membrane, and more particularly, to a method for producing a biocatalyst such as a microorganism. The present invention relates to a method for producing a hollow fiber module used as a means for producing a useful substance by utilizing the module. (Prior Art) An ultrafiltration method using a separation membrane having an ability to filter various substances by a sieving principle is widely known. FIG. 1 shows an example of a hollow fiber module using a hollow fiber type separation membrane, and a plurality of hollow fiber type separation membranes (1).
Is inserted into an outer cylinder (2) provided with an inlet (3) and an outlet (3 '), and both ends of each hollow fiber type separation membrane (1) and the outer cylinder (2) are potted with an adhesive. Member (4) provided with an inflow hole (5) and an outflow hole (5 ')
(4) covers both ends of the outer cylinder (2). The hollow fiber type separation membrane (1) is marketed in a grade having a pore size in the range of several μm to several μm.
It is widely used for various applications, and in particular, in recent years, has rapidly grown to be applied to so-called bioreactors, which produce useful substances using biocatalysts. Separation membranes in bioreactors are used for the purpose of not preserving valuable biocatalysts from the bioreactor (immobilization) and for the purpose of directly separating useful substances produced by the biocatalysts and simplifying subsequent steps. . In the bioreactor, in order to prevent the propagation of other germs, regardless of the membrane type or batch type, a sterilization operation step is performed before the start of operation, and as this sterilization operation step, usually steam sterilization is performed, This is done by exposing all wetted parts to high-temperature steam at about 120 ° C for 10 to 20 minutes. (Problems to be Solved by the Invention) In the hollow fiber module subjected to the thermal shock by the steam sterilization operation described above, the peeling phenomenon of the bonded portion and the hollow fiber type separation membrane caused by the difference in the coefficient of thermal expansion of the component parts. In some cases, the hollow fiber type separation membrane was damaged due to shrinkage of the hollow fiber type separation membrane. That is, as shown in FIG. 1, due to the difference in the coefficient of thermal expansion between the potting agent for bonding both ends of the hollow fiber type separation membrane (1) and the outer cylinder (2) and the outer cylinder (2), In some cases, the adhesive surface was peeled off due to a thermal shock, which caused a leak. The phenomenon of peeling of the adhesive surface is that the hardness of the potting agent is
The Shore D hardness is about 85, the elasticity is small, and the strain applied between the outer cylinder and the potting agent due to heating cannot be absorbed. is there. Next, the polymer-based hollow fiber type separation membrane often shrinks when exposed to a high temperature. This is presumably because the fine network structure caused by the phase separation becomes more stable, that is, denser due to thermal motion between molecules at a high temperature. Actually, an ultrafiltration membrane
Leaving in a steam atmosphere close to ° C. causes a decrease in the amount of water permeation and a shift of the fractionation curve toward the lower molecular weight side. For this purpose, as shown in FIG. 1, the hollow fiber type separation membrane (1) potted at both ends with an adhesive was exposed to steam at 120 ° C. and returned to room temperature (20 to 30 ° C.). Due to the shrinkage at the time, a stress (tension) is added, and when the tension becomes a certain level or more, fine cracks are generated on the surface of the membrane, and as a result, there is a possibility that bacterial cells leak. The present invention, in the above-described conventional hollow fiber module, suppresses the peeling phenomenon of the potting agent that causes a leak at the bonding portion to the outer cylinder, and the minute cracks in the hollow fiber type separation membrane that causes the leakage of bacterial cells. The purpose of the present invention is to present a method for producing a hollow fiber module to be obtained. (Means for Solving the Problems) The present invention takes into consideration the problems in the hollow fiber module according to the conventional manufacturing method described above, and places the hollow fiber type separation membrane in a steam atmosphere prior to insertion into the outer cylinder. To give a heat history, and then fix a large number of hollow fiber type separation membranes and the end of the outer cylinder with a potting agent, and furthermore, the potting agent has a Shore D hardness of approximately
It is a configuration that is 50 adhesives. (Function) In the method for manufacturing a hollow fiber module according to the present invention having the above-described configuration, the hollow fiber type separation membrane provided with the thermal history suppresses its own shrinkage due to the sterilization operation in steam. Shows that the slightly soft adhesive having a Shore D hardness of about 50 used for potting the hollow fiber type separation membrane and the end of the outer cylinder suppresses the peeling phenomenon of the potting portion due to sterilization in steam. (Example) Using a polysulfone hollow fiber type separation membrane and a polycarbonate module outer cylinder, as a potting agent, U-537 manufactured by Nippon Polyurethane Co., Ltd., and Millionate MTL-C
A hollow fiber module is manufactured using a combination of polyurethane (potting agent) with a curing agent of C-11A or polyurethane (potting agent) with a curing agent of N-148 as a main agent. When a heating operation in a steam atmosphere was added prior to bonding to the outer cylinder and when the heating operation was not added, the presence or absence of a leak after the steam sterilization operation was examined, and the following results were obtained. Hardness of potting agent: Shore D84 Shore D50 Heat treatment conditions: Autoclave 120 ° C, 1 atm From the test results described above, prior to the bonding step of the hollow fiber type separation membrane and the outer cylinder, impart a heat history to the hollow fiber separation membrane,
Furthermore, it has proven effective to use a low hardness adhesive as the potting agent. (Effect of the Invention) The method for manufacturing a hollow fiber module according to the present invention, as described above, exposes a hollow fiber type separation membrane to the above-described atmosphere in advance and imparts a heat history such as shrinkage of the membrane generated by high-temperature steam heating. Before use, the hollow fiber module in which the hollow fiber type separation membrane having the thermal history is incorporated and the end is fixed is heated by a high-temperature steam heating operation before use, and the thermal expansion of the outer cylinder and the hollow fiber Since the tension applied to the separation membrane caused by the contraction of the mold separation membrane can be reduced, there is an advantage that the occurrence of damage such as cracks in the hollow fiber type separation membrane can be significantly reduced. In addition, since an adhesive having a low Shore D hardness of about 50 and a low flexibility is used as a potting agent between the hollow fiber type separation membrane and the outer cylinder, heat generated between the outer cylinder and the potting agent generated during high-temperature steam treatment. Distortion due to differences in expansion can be flexibly absorbed. For this reason, the adhesive part peeling phenomenon between the outer cylinder and the potting agent or between the hollow fiber and the potting agent can be effectively suppressed. That is, the steam heating history is given to the hollow fiber type separation membrane,
Furthermore, by forming an adhesive having a Shore D hardness of approximately 50 between the potting agents, even after being subjected to a sterilization operation by being exposed to a steam atmosphere after the completion of the production, cracks and adhesion due to shrinkage of the hollow fiber type separation membrane are caused. Since no exfoliation occurs in the part, the risk of unavoidable leakage of useful substances in the hollow fiber module manufactured by the conventional method is completely eliminated.
【図面の簡単な説明】
第１図は、本発明の対象となる中空糸モジュールの一例
の断面図である。
１……中空糸型分離膜、２……外筒、３……流入口、
３′……流出口、４……蓋部材、５……流入孔、５′…
…流出孔。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a sectional view of an example of a hollow fiber module to which the present invention is applied. 1 ... hollow fiber type separation membrane, 2 ... outer cylinder, 3 ... inflow port,
3 '... outlet, 4 ... lid member, 5 ... inlet hole, 5' ...
... outflow holes.
Claims (1)
糸型分離膜の多数本及び前記外筒の端部をポッテイング
してなる中空糸モジュールの製作方法において、前記中
空糸型分離膜に高温蒸気による熱履歴を付与し、その後
前記中空糸型分離膜の多数本及び前記外筒の端部をショ
アーＤ硬度略50の接着剤でポッテイングして固定するこ
とを特長とする中空糸膜モジュールの製作方法。(57) [Claims] A method for manufacturing a hollow fiber module, comprising inserting a plurality of hollow fiber type separation membranes into an outer cylinder and potting the plurality of hollow fiber type separation membranes and the end of the outer cylinder. A hollow fiber membrane, wherein a large number of the hollow fiber type separation membranes and an end of the outer cylinder are potted and fixed with an adhesive having a Shore D hardness of about 50. How to make a module.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62260548A JP2826823B2 (en) | 1987-10-15 | 1987-10-15 | Manufacturing method of hollow fiber module |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62260548A JP2826823B2 (en) | 1987-10-15 | 1987-10-15 | Manufacturing method of hollow fiber module |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01104311A JPH01104311A (en) | 1989-04-21 |
| JP2826823B2 true JP2826823B2 (en) | 1998-11-18 |
Family
ID=17349487
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62260548A Expired - Lifetime JP2826823B2 (en) | 1987-10-15 | 1987-10-15 | Manufacturing method of hollow fiber module |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2826823B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5048189B2 (en) * | 2001-09-28 | 2012-10-17 | ダイセン・メンブレン・システムズ株式会社 | Hollow fiber membrane module |
| JP2012176345A (en) * | 2011-02-25 | 2012-09-13 | Toray Ind Inc | Spiral type fluid separation element |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6058210A (en) * | 1983-09-08 | 1985-04-04 | Toyobo Co Ltd | Preparation of cellulose ester type hollow yarn membrane |
-
1987
- 1987-10-15 JP JP62260548A patent/JP2826823B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01104311A (en) | 1989-04-21 |
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|---|---|---|---|
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