JP2993217B2 - Method for producing hollow fiber-shaped porous separation membrane element - Google Patents

Method for producing hollow fiber-shaped porous separation membrane element

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Publication number
JP2993217B2
JP2993217B2 JP3246584A JP24658491A JP2993217B2 JP 2993217 B2 JP2993217 B2 JP 2993217B2 JP 3246584 A JP3246584 A JP 3246584A JP 24658491 A JP24658491 A JP 24658491A JP 2993217 B2 JP2993217 B2 JP 2993217B2
Authority
JP
Japan
Prior art keywords
hollow fiber
porous separation
separation membrane
resin
shaped porous
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
Application number
JP3246584A
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Japanese (ja)
Other versions
JPH0557153A (en
Inventor
進一 金澤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Electric Industries Ltd
Original Assignee
Sumitomo Electric Industries Ltd
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Filing date
Publication date
Application filed by Sumitomo Electric Industries Ltd filed Critical Sumitomo Electric Industries Ltd
Priority to JP3246584A priority Critical patent/JP2993217B2/en
Publication of JPH0557153A publication Critical patent/JPH0557153A/en
Application granted granted Critical
Publication of JP2993217B2 publication Critical patent/JP2993217B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は、中空糸状多孔質分離膜
エレメントの製造方法に関し、さらに詳しくは、ガス分
離膜、透析膜、逆浸透膜、限外濾過膜、精密濾過膜など
として用いられる中空糸状多孔質分離膜を用いた耐熱
性、耐薬品性等に優れた中空糸状多孔質分離膜エレメン
トの製造方法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a hollow fiber-shaped porous separation membrane element, and more particularly, it is used as a gas separation membrane, a dialysis membrane, a reverse osmosis membrane, an ultrafiltration membrane, a microfiltration membrane, or the like. The present invention relates to a method for producing a hollow fiber-like porous separation membrane element having excellent heat resistance, chemical resistance, and the like using a hollow fiber-like porous separation membrane.

【0002】[0002]

【従来の技術】中空糸状多孔質分離膜は、中空繊維の壁
部を選択性透過膜として利用する分離膜であり、ガス分
離膜、透析膜、逆浸透膜、限外濾過膜、精密濾過膜など
に用いられている。この中空糸状多孔質分離膜は、単位
体積当たりの膜面積を増大させるために、中空糸型モジ
ュール化して実用に供している。
2. Description of the Related Art A hollow fiber type porous separation membrane is a separation membrane that uses the walls of hollow fibers as a selective permeable membrane, and is a gas separation membrane, a dialysis membrane, a reverse osmosis membrane, an ultrafiltration membrane, a microfiltration membrane. It is used for such purposes. This hollow fiber-shaped porous separation membrane has been put into practical use as a hollow fiber type module in order to increase the membrane area per unit volume.

【0003】中空糸型モジュールは、中空糸状多孔質分
離膜(中空糸)の束を円筒状等の耐圧性の外筒に収納し
たエレメントを含み、膜の充填密度が高く、例えば、
水、ジュース、酒あるいは溶剤等の液体の有用物を塵
埃、雑菌等から分離する濾過装置の小型化を計ることが
できる他、耐圧性に優れているため、半導体、食品、そ
の他の分野で多く用いられている。特に、フッ素樹脂な
どの疎水性樹脂からなる中空糸状多孔質分離膜は、耐薬
品性に優れていることから賞用されている。
The hollow fiber module includes an element in which a bundle of hollow fiber porous separation membranes (hollow fibers) is housed in a pressure-resistant outer cylinder such as a cylinder, and has a high packing density of the membrane.
It can be used to reduce the size of filtration equipment that separates liquid useful substances such as water, juice, alcohol, and solvents from dust, germs, etc., and because of its excellent pressure resistance, it is often used in the semiconductor, food, and other fields. Used. In particular, a hollow fiber-shaped porous separation membrane made of a hydrophobic resin such as a fluororesin has been awarded due to its excellent chemical resistance.

【0004】中空糸型モジュールにおいては、多数の中
空糸状多孔質分離膜の束を円筒等の外筒に収納したエレ
メントを用いており、中空糸状多孔質分離膜の一端を熱
融着封止した閉鎖型の内圧式分離膜エレメントや両端の
開口部を開放した内圧循環式分離膜エレメントなどがあ
る。これらのエレメントでは、多数の中空糸状多孔質分
離膜の束を外筒に収納し、その一端または両端部におい
て、中空糸状多孔質分離膜相互の間隙および中空糸状多
孔質分離膜と外筒の間隙を封止剤等で封止している。
[0004] The hollow fiber type module uses an element in which a bundle of a large number of hollow fiber-shaped porous separation membranes is housed in an outer cylinder such as a cylinder, and one end of the hollow fiber-shaped porous separation membrane is heat-sealed and sealed. There are a closed internal pressure type separation membrane element and an internal pressure circulation type separation membrane element having openings at both ends. In these elements, a bundle of a large number of hollow fiber-like porous separation membranes is housed in an outer cylinder, and at one or both ends thereof, a gap between the hollow fiber-like porous separation membranes and a gap between the hollow fiber-like porous separation membrane and the outer cylinder are provided. Is sealed with a sealant or the like.

【0005】従来、外筒と中空糸束との間隙や中空糸束
相互の間隙を封止する方法として、封止剤としてエポキ
シ樹脂、ウレタン樹脂、シリコーン樹脂等の低粘度の樹
脂を端末部に注入し、静置あるいは遠心力により、間隙
に充分充填させた後、加熱硬化させる方法が知られてい
る(特公昭44−5526号、特公昭56−40602
号)。
Conventionally, as a method of sealing the gap between the outer cylinder and the hollow fiber bundle or the gap between the hollow fiber bundles, a low-viscosity resin such as an epoxy resin, a urethane resin, or a silicone resin is used as a sealant at the terminal. A method is known in which the material is injected, allowed to stand still or centrifugal force to sufficiently fill the gap, and then heated and cured (JP-B-44-5526, JP-B-56-40602).
issue).

【0006】ところが、封止剤として使用するこれらの
樹脂は、耐熱性や耐薬品性の点で充分ではなく、酸やア
ルカリを含む溶液または有機溶剤を溶媒や洗浄液として
使用したり、あるいは蒸気滅菌したりする分野に適用す
るには、制限があった。すなわち、エポキシ樹脂は、比
較的耐熱性に優れているものの、強酸、強アルカリおよ
び一部の溶剤にもろく、また、皮膚感作性があり、薬品
や食品分野への適用は制限される。ウレタン樹脂は、耐
熱性が不充分であり、しかも強酸、強アルカリおよび一
部の溶剤に耐性を持たない。シリコーン樹脂は、耐溶剤
性に劣る。
However, these resins used as sealants are not sufficient in terms of heat resistance and chemical resistance, and a solution or an organic solvent containing an acid or an alkali is used as a solvent or a cleaning solution, or steam sterilization. There was a limit to applying to the fields that do. That is, although the epoxy resin is relatively excellent in heat resistance, it is fragile to strong acids, strong alkalis and some solvents, has skin sensitization, and its application in the field of medicine and food is limited. Urethane resins have insufficient heat resistance and do not have resistance to strong acids, strong alkalis and some solvents. Silicone resins have poor solvent resistance.

【0007】一方、中空糸状多孔質分離膜エレメントの
封止剤として熱溶融性樹脂を使用する場合には、(1)
中空糸束を収納した外筒を型内に配置し、樹脂を加熱溶
融して流し込む射出成型または押出成型による方法、
(2)中空糸束を収納した外筒を型内に配置し、粉状、
粒状またはペレット状の樹脂を型に入れて加熱溶融し、
樹脂中に含まれる気泡を脱泡する方法、(3)予め蜂の
巣状の貫通孔を有する樹脂を成型し、中空糸を孔中に装
着してから熱溶融する方法等がある。
On the other hand, when a hot-melt resin is used as a sealant for a hollow fiber-shaped porous separation membrane element, (1)
A method of injection molding or extrusion molding in which an outer cylinder containing a hollow fiber bundle is placed in a mold, and the resin is heated and melted and poured.
(2) Placing the outer cylinder containing the hollow fiber bundle in the mold,
Put the granular or pellet resin into the mold and heat and melt,
There are a method of defoaming bubbles contained in the resin, a method of (3) molding a resin having a honeycomb-shaped through hole in advance, mounting a hollow fiber in the hole, and then thermally melting the resin.

【0008】しかしながら、(1)の方法では、熱溶融
性樹脂の粘度が高い場合には、外筒と中空糸束や中空糸
束相互の間隙などの細い間隙に樹脂を侵入させることが
困難である。(2)の方法では、一度入った気泡を高粘
度の樹脂から抜くことは困難であり、封止が不完全とな
る。(3)の方法では、多数の貫通孔を高密度で作成す
ること自体が困難であるとともに、気泡の混入が避けら
れず、しかも間隙を完全に封止することが難しい。した
がって、これらの方法によっては、熱溶融性樹脂を用い
て封止部を微細成型することができず、中空糸の充填率
を上げることもできない。
However, in the method (1), when the viscosity of the hot-melt resin is high, it is difficult to make the resin penetrate into narrow gaps such as the gap between the outer cylinder and the hollow fiber bundle or between the hollow fiber bundles. is there. In the method (2), it is difficult to remove air bubbles that have entered once from the high-viscosity resin, resulting in incomplete sealing. In the method (3), it is difficult to form a large number of through holes at a high density, and it is inevitable to mix air bubbles, and it is difficult to completely seal the gap. Therefore, according to these methods, the sealing portion cannot be finely molded using the heat-fusible resin, and the filling rate of the hollow fiber cannot be increased.

【0009】中空糸状多孔質分離膜エレメントの最大の
長所は、単位体積当たりの膜面積を増大できることであ
るが、そのためには、外筒内に中空糸を高度に充填する
ことが不可欠であり、中空糸の充填率(エレメント内体
積に対する、中空糸の内腔を含む体積の合計の割合)は
一般に50%以上とする必要があるとされている。しか
し、封止剤として熱溶融性樹脂を用い高充填率の中空糸
状多孔質分離膜エレメントを作成することは極めて困難
である。特に、耐熱性や耐薬品性に優れた熱溶融性樹脂
は、一般に高融点・高粘度であるため、従来公知の成型
法により封止剤として使用することは、実際には無理で
あった。
[0009] The greatest advantage of the hollow fiber-shaped porous separation membrane element is that the membrane area per unit volume can be increased. For that purpose, it is essential to highly fill the outer cylinder with the hollow fiber, It is generally said that the filling rate of the hollow fiber (the ratio of the total volume including the lumen of the hollow fiber to the volume of the element) needs to be 50% or more. However, it is extremely difficult to prepare a hollow fiber-shaped porous separation membrane element having a high filling rate by using a heat-meltable resin as a sealing agent. Particularly, since a heat-meltable resin having excellent heat resistance and chemical resistance generally has a high melting point and a high viscosity, it was actually impossible to use it as a sealant by a conventionally known molding method.

【0010】[0010]

【発明が解決しようとする課題】本発明の目的は、耐熱
性、耐薬品性が大幅に改善された高充填率の中空糸状多
孔質分離膜エレメントの製造方法を提供することにあ
る。また、本発明の目的は、熱溶融性フッ素樹脂等の熱
溶融性樹脂を用いて、中空糸状多孔質分離膜エレメント
の末端封止部を形成させる工程を含む中空糸状多孔質分
離膜エレメントの製造方法を提供することにある。
SUMMARY OF THE INVENTION It is an object of the present invention to provide a method for producing a hollow fiber-like porous separation membrane element having a high filling factor and significantly improved heat resistance and chemical resistance. Further, an object of the present invention is to manufacture a hollow fiber-shaped porous separation membrane element including a step of forming a terminal sealing portion of a hollow fiber-shaped porous separation membrane element using a heat-meltable resin such as a heat-meltable fluororesin. It is to provide a method.

【0011】熱溶融性フッ素樹脂は、耐熱、耐薬品性に
優れているが、一般に高融点・高粘度であるため、前記
した射出成型法、押出成型法、粉末成型法などによっ
て、中空糸状多孔質分離膜エレメントの末端封止部を形
成させることは極めて困難であり、満足のいく製品を得
ることはできない。例えば、FEP(テトラフルオロエ
チレン/ヘキサフルオロプロピレン共重合体)の成型用
樹脂の比溶融粘度は、通常、104〜106ポアズと高
く、溶融させても加圧なしではほとんど流動性はない。
したがって、熱溶融性フッ素樹脂を中空糸状多孔質分離
膜エレメントの末端封止用の封止剤として使用するに
は、細かい隙間に樹脂を侵入させるために高圧が必要で
あり、従来の成型技術では事実上不可能であると考えら
れていた。
Although the heat-meltable fluororesin is excellent in heat resistance and chemical resistance, it generally has a high melting point and a high viscosity. It is extremely difficult to form an end seal of a quality separation membrane element, and a satisfactory product cannot be obtained. For example, the specific melting viscosity of a molding resin of FEP (tetrafluoroethylene / hexafluoropropylene copolymer) is generally as high as 10 4 to 10 6 poise, and there is almost no fluidity without melting even if it is melted.
Therefore, in order to use a hot-melt fluororesin as a sealant for sealing the end of a hollow fiber-shaped porous separation membrane element, high pressure is required to allow the resin to penetrate into fine gaps, and conventional molding techniques require It was thought to be virtually impossible.

【0012】このように、中空糸状多孔質分離膜相互の
間隙および中空糸状多孔質分離膜と外筒との間隙という
微細な形状部分に高粘度の熱溶融性樹脂を侵入させて末
端封止部を形成することは、極めて困難であるか、ある
いは不可能であると考えられていた。これに対して、本
発明者は、従来の発想とは逆に、中空糸状多孔質分離膜
相互の間隙を疎にした状態でその間隙を熱溶融性樹脂で
埋め、ついで熱溶融性樹脂を加熱溶融しながら圧縮する
と、熱溶融性樹脂で末端封止部が形成され、かつ、高充
填率の中空糸状多孔質分離膜エレメントの得られること
を見出した。本発明は、これらの知見に基づいて完成す
るに至ったものである。
As described above, the highly viscous heat-meltable resin penetrates into the finely shaped portions such as the gaps between the hollow fiber-shaped porous separation membranes and the gaps between the hollow fiber-shaped porous separation membranes and the outer cylinder, so that the end sealing portion is formed. Was thought to be extremely difficult or impossible. On the other hand, the present inventor, contrary to the conventional idea, fills the gaps between the hollow fiber-shaped porous separation membranes with the heat-meltable resin in a state where the gaps are sparse, and then heats the heat-meltable resin. It has been found that when melted and compressed, a terminal sealing portion is formed with a hot-melt resin, and a hollow fiber-shaped porous separation membrane element having a high filling rate can be obtained. The present invention has been completed based on these findings.

【0013】[0013]

【課題を解決するための手段】かくして本発明によれ
ば、多数の中空糸状多孔質分離膜の一端を熱溶融性樹脂
中に挿入した形状の予備成型物を作成し、ついで該予備
成型物の熱溶融性樹脂を加熱して溶融状態にしながら周
囲から加圧することにより、各中空糸状多孔質分離膜相
互の間隙を減少させて、所望形状の熱溶融性樹脂からな
る末端封止部を形成させることを特徴とする中空糸状多
孔質分離膜エレメントの製造方法が提供される。
Thus, according to the present invention, a preform having a shape in which one end of a number of hollow fiber-like porous separation membranes is inserted into a hot-melt resin is prepared, and then the preform is formed. By applying pressure from the surroundings while heating and melting the hot-melt resin, the gap between the hollow fiber-shaped porous separation membranes is reduced, and the end sealing portion made of the hot-melt resin having a desired shape is formed. A method for producing a hollow fiber-shaped porous separation membrane element is provided.

【0014】以下、本発明について詳述する。本発明の
技術思想の根本は、中空糸状多孔質分離膜と封止剤を作
成しやすい低充填率で一体化させた後に、これを絞り込
んで高密度化することにある。
Hereinafter, the present invention will be described in detail. The root of the technical idea of the present invention is to integrate the hollow fiber-shaped porous separation membrane and the sealing agent at a low filling rate that is easy to produce, and then to narrow down the density to increase the density.

【0015】本発明の製造方法について図面を参照しな
がら説明する。図1に示すように、最初に、低充填率の
中空糸状多孔質分離膜1と熱溶融性樹脂からなる封止剤
2とが一体になった端末部を形成する。この場合、中空
糸状多孔質分離膜の形状を保持するためにステンレス等
の金属やセラミックス等の耐熱性の材質からなる支え棒
6を内腔に挿入しておく。ついで、熱溶融性樹脂を加熱
して溶融状態にし、図1の矢印で示すように、周囲から
加圧することにより熱溶融性樹脂を圧縮し、全体を絞り
込むようにすると、図2に示すように、中空糸状多孔質
分離膜の充填密度が向上し、かつ、稠密な末端封止部が
形成される。
The manufacturing method of the present invention will be described with reference to the drawings. As shown in FIG. 1, first, a terminal portion in which a hollow fiber-shaped porous separation membrane 1 having a low filling rate and a sealant 2 made of a hot-melt resin are integrated is formed. In this case, a support rod 6 made of a heat-resistant material such as a metal such as stainless steel or ceramics is inserted into the lumen in order to maintain the shape of the hollow fiber-shaped porous separation membrane. Then, the hot-melt resin is heated to a molten state, and as shown by the arrow in FIG. 1, the hot-melt resin is compressed by being pressed from the surroundings and the whole is narrowed down, as shown in FIG. As a result, the packing density of the hollow fiber-shaped porous separation membrane is improved, and a dense end sealing portion is formed.

【0016】予め低充填率の中空糸状多孔質分離膜と封
止剤が一体になった端末部を有する予備成型物を形成す
る方法としては、(1)中空糸状多孔質分離膜の一端を
これが挿入できる穴を持つ熱溶融性樹脂成型物(例えば
チューブ状の成型物)に挿入したものを多数束ねる方
法、(2)中空糸状多孔質分離膜の一端をこれが挿入で
きる穴を多数持つ熱溶融性樹脂成型物に多数挿入する方
法、あるいは(3)多数の中空糸状多孔質分離膜の間隙
に熱溶融性樹脂を加熱溶融して流し込む射出成型または
押出成型による方法、(4)中空糸状多孔質分離膜束を
収納した型内に、粉状、粒状またはペレット状の熱溶融
性樹脂を入れて加熱溶融する方法、などが挙げられる。
これらの中でも、熱溶融樹脂成型物を形成しておく
(1)〜(2)の方法が、操作が容易で、樹脂中への気
泡の封入がない点で特に好ましい。
The method of forming a preform having a terminal portion in which a hollow fiber-shaped porous separation membrane having a low filling factor and a sealing agent are integrated in advance is as follows: (1) One end of the hollow fiber-shaped porous separation membrane is A method of bundling a large number of heat-fusible resin molded products (for example, tube-shaped molded products) having holes that can be inserted, and (2) a heat-fusible resin having many holes into which one end of a hollow fiber-shaped porous separation membrane can be inserted. A method of inserting a large number into a resin molded product, or (3) a method of injection molding or extrusion molding in which a hot-melt resin is melted and poured into the gaps of a large number of hollow fiber-like porous separation membranes, (4) hollow fiber-like porous separation A method in which a powdery, granular, or pellet-like heat-fusible resin is put into a mold containing a film bundle and then heated and melted is used.
Among these, the methods (1) and (2), in which a hot-melt resin molded product is formed, are particularly preferable because they are easy to operate and do not enclose air bubbles in the resin.

【0017】これら予備成型物を形成する方法は、従来
法とは異なり、中空糸状多孔質分離膜相互の間隙が比較
的大きいため、容易に実施することができる。ただし、
予備成型物で使用する中空糸状多孔質分離膜の本数は、
最終的な充填率に必要な数とする。
Unlike the conventional method, the method of forming these preforms can be easily carried out because the gap between the hollow fiber-like porous separation membranes is relatively large. However,
The number of hollow fiber-shaped porous separation membranes used in the preform is
Number required for final filling rate.

【0018】予備成型物においては、末端封止部を形成
する部分の断面積が大きなものとなっており、しかも空
隙または気泡を含んでいる場合がある。これを絞り込ん
で所望の断面積と形状を有する緻密な末端封止部を形成
するには、例えば、図3に示すような装置を用いる。
In the preform, the cross-sectional area of the portion forming the end sealing portion is large, and may contain voids or air bubbles. In order to form a dense end sealing portion having a desired cross-sectional area and shape by narrowing this, for example, an apparatus as shown in FIG. 3 is used.

【0019】図3の受け部4の凹部に予備成型物を挿入
し、加熱して熱溶融性樹脂(封止剤)を溶融状態にしな
がら、移動部3に圧力を加えて熱溶融性樹脂を絞り込む
と、図4に示すように、末端封止部の断面積が縮小され
る。封止剤を加熱溶融させながら、加圧成形して目的の
大きさに縮小する。つまり、分離膜間の封止剤を絞り込
んでいくわけである。この際、絞り出された封止剤の逃
げる場所を設ける必要があるが、これは加圧装置の周壁
に孔を設けておくか、あるいは加圧の際に上部や下部に
逃げていく封止剤の量を考慮して、予備成型物における
封止剤の高さを最終的な所望の高さより低くしておいて
もよい。
The preform is inserted into the concave portion of the receiving portion 4 shown in FIG. 3, and while the hot melt resin (sealing agent) is in a molten state by heating, pressure is applied to the moving portion 3 to remove the hot melt resin. When narrowing down, as shown in FIG. 4, the cross-sectional area of the end sealing portion is reduced. While the sealant is being heated and melted, it is molded under pressure to reduce it to a desired size. That is, the sealant between the separation membranes is narrowed down. At this time, it is necessary to provide a place where the squeezed sealant escapes, but this can be done by providing a hole in the peripheral wall of the pressurizing device, or by sealing up or down at the time of pressurization. In consideration of the amount of the agent, the height of the sealant in the preform may be lower than the final desired height.

【0020】この方法によれば、元々全く一体化した低
充填率の端末部を作成しなくとも、例えば、封止剤のチ
ューブ状ないしはパイプ状のものを分離膜の端部に被せ
て、これを多数本束ねた状態で絞り込んでも、封止剤同
士や封止剤と分離膜の間に発生する隙間や気泡は絞り込
みによって上へ逃げていくので、最終的には一体化が可
能である。この方法は、簡便で手間がかからず有用であ
る。
According to this method, for example, a tube-shaped or pipe-shaped sealant may be covered on the end of the separation membrane without forming a terminal part having a low filling rate which is completely integrated originally. Even if a large number of are bundled together, the gaps and bubbles generated between the sealants or between the sealant and the separation membrane escape upward by the narrowing, so that they can be finally integrated. This method is simple, convenient, and useful.

【0021】かくして得られた末端封止部を有する中空
糸束は、中空糸状多孔質分離膜エレメントとするため
に、通常、図5に示すように外筒5中に挿入し、ついで
端部を切断し(図6)、支え棒を抜き去ってエレメント
とする(図7)。このエレメントにおいては、中空糸状
多孔質分離膜相互の微細な間隙および中空糸状多孔質分
離膜と外筒との微細な間隙に熱溶融性樹脂が侵入した形
状の末端封止部が形成されている(図8)。
The thus obtained hollow fiber bundle having a terminal sealing portion is usually inserted into an outer cylinder 5 as shown in FIG. 5 in order to form a hollow fiber-like porous separation membrane element, and then the end portion is formed. It is cut (FIG. 6) and the support rod is pulled out to make an element (FIG. 7). In this element, an end sealing portion having a shape in which a hot-melt resin invades a minute gap between the hollow fiber-shaped porous separation membranes and a minute gap between the hollow fiber-shaped porous separation membrane and the outer cylinder is formed. (FIG. 8).

【0022】本発明で使用する中空糸状多孔質分離膜
は、特に限定されないが、特に、PTFE(ポリテトラ
フルオロエチレン)製中空糸などフッ素樹脂製のものが
好適に使用できる。また、円筒状などのエレメント外筒
の材質としては、耐熱性、耐薬品性に優れたステンレス
等の金属やPTFE、FEP、PFA(テトラフルオロ
エチレン/パーフルオロアルキルビニルエーテル共重合
体)などのフッ素樹脂が好ましい。
The hollow fiber-like porous separation membrane used in the present invention is not particularly limited, but in particular, one made of a fluororesin such as PTFE (polytetrafluoroethylene) hollow fiber can be suitably used. Examples of the material of the element outer cylinder such as a cylindrical shape include metals such as stainless steel having excellent heat resistance and chemical resistance, and fluorine resins such as PTFE, FEP, and PFA (tetrafluoroethylene / perfluoroalkylvinyl ether copolymer). Is preferred.

【0023】本発明において封止剤として使用される熱
溶融性樹脂としては、例えば、FEP、PFA、ETF
E(エチレン/テトラフルオロエチレン共重合体)、P
CTFE(ポリクロロトリフルオロエチレン)、PVd
F(ポリビニリデンフルオライド)等の熱溶融性フッ素
樹脂を挙げることができる。これらの中でも、蒸気滅菌
への耐性を基準にした耐熱性と、酸、アルカリおよび溶
剤に対する耐薬品性の観点から、FEPとPFAが最も
適している。
The hot-melt resin used as a sealant in the present invention includes, for example, FEP, PFA, ETF
E (ethylene / tetrafluoroethylene copolymer), P
CTFE (polychlorotrifluoroethylene), PVd
A heat-fusible fluororesin such as F (polyvinylidene fluoride) can be used. Among them, FEP and PFA are most suitable from the viewpoint of heat resistance based on the resistance to steam sterilization and chemical resistance to acids, alkalis and solvents.

【0024】また、フッ素樹脂製の中空糸状多孔質分離
膜と封止剤として用いる熱溶融性樹脂は、親和性が高い
組合わせのもの程良く、同種の樹脂とすることが望まし
い。例えば、PTFE中空糸を使用した場合、封止剤と
しては、FEPやPFAが最適である。異種、異性質の
組み合わせの時は、中空糸表面を処理してできるだけ親
和性を上げることが望ましい。
The combination of a fluororesin hollow fiber-shaped porous separation membrane and a hot-melt resin used as a sealant is preferably as high as possible in combination, and is preferably the same kind of resin. For example, when PTFE hollow fiber is used, FEP or PFA is most suitable as a sealant. In the case of a combination of different types and isomers, it is desirable to treat the surface of the hollow fiber to increase the affinity as much as possible.

【0025】本発明の製造方法による中空糸状多孔質分
離膜エレメントは、従来品と同様の50〜60%の中空
糸充填率を保持することができる。
The hollow fiber-like porous separation membrane element produced by the production method of the present invention can maintain the same hollow fiber filling ratio of 50 to 60% as the conventional product.

【0026】本発明による製造方法は、次の点で従来の
方法よりも優れている。 (1)熱溶融性樹脂を予めチューブ状などの穴を持つ成
型物に成型することは容易である。また、予め蜂の巣状
の貫通孔を有する樹脂を成型する場合にも、円柱状また
は平板状の熱溶融性樹脂の成型物に低密度で孔を開ける
だけなので、簡便であるため高粘度の熱溶融性樹脂でも
成型が容易である。
The manufacturing method according to the present invention is superior to the conventional method in the following points. (1) It is easy to mold the hot-melt resin into a molded article having a hole such as a tube in advance. Also, when molding a resin having a honeycomb-shaped through-hole in advance, holes are formed at a low density in a cylindrical or flat-shaped molded resin of the heat-meltable resin. Molding is easy even with conductive resins.

【0027】(2)封止剤の熱溶融性樹脂を予めバルク
状から加工・成型すると、気泡がなく封止が完全であ
る。また、加熱・加圧成型により、気泡や空隙をなくす
ことが可能である。
(2) If the heat-meltable resin of the sealing agent is previously processed and molded from a bulk state, the sealing is complete without bubbles. In addition, bubbles and voids can be eliminated by heating and pressing.

【0028】(3)封止成型する際に、高粘度で流動性
の乏しい樹脂に圧力を加えて微細な孔に侵入させるので
なく、中空糸と樹脂の一体物に加熱下で圧力をかけて、
いわば変形させるだけなので、高圧や強い力は必要がな
い。
(3) At the time of sealing and molding, instead of applying pressure to a resin having a high viscosity and poor fluidity to cause it to penetrate into fine pores, a pressure is applied to an integrated body of the hollow fiber and the resin under heating. ,
There is no need for high pressure or strong force, as it only deforms.

【0029】したがって、本発明の製造方法において
は、従来、高粘度であるため微細成型が困難であるとさ
れていた熱溶融性フッ素樹脂を、中空糸状多孔質分離膜
エレメント末端の封止剤に使用することができるため、
従来使用されていたエポキシ樹脂、シリコーン樹脂、ウ
レタン樹脂等を封止剤としたものと比べて耐熱性、耐薬
品性を大きく改善することができる。そして、特に、熱
溶融性樹脂として、FEPやPFAを用いると、強酸
性、強アルカリ性の溶液またはあらゆる溶剤を溶媒とす
る分離・濃縮用途に使用可能であり、また、蒸気滅菌を
繰り返し行なうことが可能な中空糸状多孔質分離膜エレ
メントが得られる。
Therefore, in the production method of the present invention, a heat-meltable fluororesin, which has conventionally been considered to be difficult to finely mold due to its high viscosity, is used as a sealant at the end of the hollow fiber-shaped porous separation membrane element. Can be used,
The heat resistance and the chemical resistance can be greatly improved as compared with a conventionally used epoxy resin, silicone resin, urethane resin or the like using a sealing agent. In particular, when FEP or PFA is used as the hot-melt resin, it can be used for separation and concentration using a strongly acidic or strongly alkaline solution or any solvent as a solvent, and can be repeatedly subjected to steam sterilization. A possible hollow fiber-like porous separation membrane element is obtained.

【0030】[0030]

【実施例】以下、本発明について、実施例および比較例
を挙げて具体的に説明するが、本発明は、これらの実施
例のみに限定されるものではない。
EXAMPLES Hereinafter, the present invention will be described specifically with reference to Examples and Comparative Examples, but the present invention is not limited to only these Examples.

【0031】[実施例1]中空糸状多孔質分離膜とし
て、気孔率65%、平均孔径0.8μm、内径2mm、
外径3mmのPTFE(ポリテトラフルオロエチレン)
多孔質チューブを用いた。末端封止剤として、FEP
(テトラフルオロエチレン/ヘキサフルオロプロピレン
共重合体)からなる95mm×95mmの正方形に95
mmφの半円を左右にくっつけた形(小判形)で高さ1
0mmの成型物を用意し、このFEP成形物の小判形の
面に垂直に、3mmφの貫通孔をほぼ均一に630個開
けた。
Example 1 As a hollow fiber-shaped porous separation membrane, a porosity of 65%, an average pore diameter of 0.8 μm, and an inner diameter of 2 mm were used.
PTFE (polytetrafluoroethylene) with an outer diameter of 3 mm
A porous tube was used. FEP as terminal sealant
A 95 mm × 95 mm square made of (tetrafluoroethylene / hexafluoropropylene copolymer)
mmφ semicircle attached to the left and right (oval shape) and height 1
A 0 mm molded product was prepared, and 630 3 mmφ through-holes were formed almost uniformly perpendicular to the oval surface of the FEP molded product.

【0032】一方、PTFEチューブは、その内腔に2
mmφのステンレス製(SUS304)を挿入し、両端
を針金で縛って封止したものを630本を用意して、F
EP成形物の孔に挿入し、ちょうど剣山に花をさしたよ
うな状態にした。
On the other hand, the PTFE tube has two lumens inside.
A stainless steel (SUS304) having a diameter of mmφ was inserted, and both ends were tied up with wires and sealed.
It was inserted into the hole of the EP molded product, and it was made to look like a flower just on the mountain.

【0033】このPTFEチューブ/FEP一体品(予
備成型物)を図3の形状の金属製装置の凹部に入れて、
これを290℃に加熱した。FEPが溶融状態になった
ところで、移動部3を徐々に約6時間かけて移動させ、
最終的に図4に示すように、PTFEチューブ/FEP
一体品を小判形から95mmφの円形に変形させた。こ
の操作をチューブ両端について行なった後に、内径95
mmφのステンレス製のエレメント外筒にこれを挿入し
た。
This PTFE tube / FEP integrated product (preformed product) is put into a concave portion of a metal device having a shape shown in FIG.
This was heated to 290 ° C. When the FEP is in a molten state, the moving section 3 is gradually moved for about 6 hours,
Finally, as shown in FIG. 4, the PTFE tube / FEP
The integrated product was transformed from an oval shape to a 95 mmφ circle. After performing this operation for both ends of the tube,
This was inserted into a stainless steel element outer cylinder of mmφ.

【0034】封止部端部が外筒から少しはみ出た状態に
して、外筒を加熱しFEPと融着させた(図5)。その
後、外筒からはみ出ている部分を切断除去し(図6)、
内部のステンレス棒を引き抜いた(図7)。同様に他端
も成形し、クロスフロー方式の内圧式中空糸状多孔質分
離膜エレメントを製造した。
With the end of the sealing portion slightly protruding from the outer cylinder, the outer cylinder was heated and fused with FEP (FIG. 5). Then, the portion protruding from the outer cylinder is cut and removed (FIG. 6),
The internal stainless steel rod was pulled out (FIG. 7). Similarly, the other end was formed to produce a cross-flow type internal pressure type hollow fiber porous separation membrane element.

【0035】[実施例2]端末封止剤として、内径3m
mφ、外径4mmφ、長さ15mmのFEPチューブを
使用し、これを実施例1と同様のステンレス棒挿入PT
FE多孔質チューブの端部に被せたものを600本束ね
て使用した以外は、実施例1と同様にしてクロスフロー
方式の内圧式中空糸状多孔質分離膜エレメントを作製し
た。
Example 2 3 m inner diameter was used as a terminal sealant.
A FEP tube having a diameter of 4 mm, an outer diameter of 4 mm, and a length of 15 mm was used.
A cross-flow type internal pressure type hollow fiber-like porous separation membrane element was produced in the same manner as in Example 1, except that 600 FE porous tubes were bundled and used at the ends.

【0036】以上の実施例1および実施例2で得られた
エレメントは、その末端封止部の樹脂に気泡は見られ
ず、封止樹脂と中空糸および外筒との接着性も良好であ
った。また、中空糸内腔への封止樹脂の侵入はなかっ
た。
In the elements obtained in Examples 1 and 2 above, no bubbles were observed in the resin at the end sealing portion, and the adhesion between the sealing resin and the hollow fiber and the outer cylinder was good. Was. In addition, there was no penetration of the sealing resin into the hollow fiber lumen.

【0037】[比較例1]中空糸状多孔質分離膜、エレ
メント外筒、ステンレス棒は実施例1と同様のものを使
用した。ステンレス棒を中空糸状多孔質分離膜内腔に挿
入し、両端を針金で固定して586本束ねたものを、内
径95mmφ×10mm高の受け皿に垂直に立てたエレ
メント外筒内に入れた。その際、予め外筒内には底から
80mmの高さになるように粉状FEP(ダイキン社
製、ネオフロンFEP)を入れたおいた。この状態で3
00℃の熱風恒温槽に入れ、1週間放置した後、室温に
戻し、受け皿を取り除きエレメント外筒よりはみ出てい
るFEP部分を切断除去し、挿入したステンレス棒を抜
き去った。
[Comparative Example 1] The same hollow fiber-shaped porous separation membrane, element outer cylinder and stainless steel rod as in Example 1 were used. A stainless steel rod was inserted into the hollow fiber-shaped porous separation membrane lumen, and 586 bundled with both ends fixed with wires were placed in an element outer cylinder which was set upright on a pan with an inner diameter of 95 mmφ × 10 mm height. At that time, powder FEP (manufactured by Daikin, NEOFLON FEP) was previously placed in the outer cylinder so as to have a height of 80 mm from the bottom. 3 in this state
After placing in a hot air thermostat at 00 ° C. and allowed to stand for one week, the temperature was returned to room temperature, the tray was removed, the FEP portion protruding from the element outer cylinder was cut off, and the inserted stainless steel rod was removed.

【0038】中空糸の他端を熱融着させて封止し、さら
に、熱融着端側の外筒をステンレス製の蓋で密封して、
閉鎖型の中空糸状多孔質分離膜エレメントを得た。得ら
れた中空糸状多孔質分離膜エレメントは、その末端封止
部の樹脂に多数の気泡が見られ、中空糸相互または中空
糸と外筒との間隙に全く封止樹脂のない部分があった。
The other end of the hollow fiber is heat-sealed and sealed, and the outer cylinder at the heat-sealed end is sealed with a stainless steel lid.
A closed hollow fiber-shaped porous separation membrane element was obtained. In the obtained hollow fiber-shaped porous separation membrane element, a large number of bubbles were observed in the resin at the terminal sealing portion, and there was a portion without any sealing resin in the hollow fibers or between the hollow fibers and the outer cylinder. .

【0039】[比較例2]末端封止剤として、95mm
φ×40mm高の円柱状のFEP樹脂成形物を使用し
た。これをバイスで固定し、ドリル(ドリル刃径、2.
8mm)で蜂の巣状(レンコン状)に586本の貫通孔
を開けることを試みたが、孔と孔がつながった部分が多
数発生した。この孔に、2mmφステンレス棒を挿入・
固定した中空糸状多孔質分離膜を586本挿入した後、
受け皿をつけて、垂直に立てたエレメント外筒内にいれ
た。
Comparative Example 2 95 mm
A cylindrical FEP resin molding having a height of φ × 40 mm was used. This is fixed with a vise and a drill (drill blade diameter, 2.
Attempting to open 586 through-holes in a honeycomb shape (lotus-shaped) at 8 mm), a number of portions where the holes were connected were generated. Insert a 2mmφ stainless steel rod into this hole.
After inserting 586 fixed hollow fiber-shaped porous separation membranes,
With the pan attached, it was placed in the vertical element outer cylinder.

【0040】外筒および受け皿をバンドヒーターで30
0℃に加熱して、FEP成型物を溶融状態とした。バン
ドヒーターを切り、室温に戻るまで自然放置した。その
後、受け皿をはずして、外筒よりはみ出ているFEP成
型品部分および中空糸内腔にステンレス棒を挿入した中
空糸端部を外筒端面で切断除去し、挿入したステンレス
棒を抜き去った。得られた中空糸状多孔質分離膜エレメ
ントは、その末端封止部の樹脂に多数の気泡が見られ、
中空糸相互または中空糸と外筒との間隙に全く封止樹脂
のない部分があった。
The outer cylinder and the pan are heated with a band heater for 30 minutes.
By heating to 0 ° C., the FEP molded product was brought into a molten state. The band heater was turned off and allowed to stand naturally until it returned to room temperature. After that, the tray was removed, the FEP molded part protruding from the outer cylinder and the end of the hollow fiber in which the stainless steel rod was inserted into the hollow fiber lumen were cut off at the outer cylinder end face, and the inserted stainless steel rod was pulled out. In the obtained hollow fiber-shaped porous separation membrane element, a large number of bubbles are seen in the resin of the terminal sealing portion,
There were portions where no sealing resin was present between the hollow fibers or between the hollow fibers and the outer cylinder.

【0041】[比較例3]内径95mm、深さ20mm
の受け皿の側面に10mmφの孔をあけたものを受け皿
として使用し、実施例1と同様の中空糸状多孔質分離
膜、ステンレス棒および外筒をセットした。
Comparative Example 3 Inner diameter 95 mm, depth 20 mm
A hole having a diameter of 10 mm was formed on the side surface of the receiving pan of Example 1 and used as a receiving pan, and the same hollow fiber-shaped porous separation membrane, stainless steel rod, and outer cylinder as in Example 1 were set.

【0042】外筒および受け皿を300℃に加温しなが
ら、10mmφのパイプで受け皿と接続した溶融押出機
から、溶融状態のFEP樹脂を受け皿および外筒内に注
入した。注入は、全354ml(95mmφ×50mm
相当)を約1時間で行った。終了後、さらに24時間、
300℃に保持し、受け皿をはずした後は比較例2と同
様にしたが、FEP樹脂は中空糸間および外筒の受け皿
の孔と反対の端には注入されておらず、満足な末端封止
部は作製できなかった。
While the outer cylinder and the tray were heated to 300 ° C., a molten FEP resin was injected into the tray and the outer cylinder from a melt extruder connected to the tray with a 10 mmφ pipe. The injection was 354 ml in total (95 mmφ × 50 mm
Equivalent) in about 1 hour. After finishing, another 24 hours,
After maintaining the temperature at 300 ° C. and removing the pan, the same operation as in Comparative Example 2 was carried out, but the FEP resin was not injected between the hollow fibers and the end of the outer cylinder opposite to the hole of the pan. The stop could not be made.

【0043】[比較例4]実施例1と同様の中空糸状多
孔質分離膜を用いて、以下の工程で末端封止部がエポキ
シ樹脂製のエレメントを作成した。中空糸状多孔質分離
膜586本の両端を熱融着封止し、フッ素樹脂表面改質
剤(潤工社製、テトラエッチ)にてその端の3〜5cm
を処理した後、FEPの代わりにエポキシ樹脂(チバガ
イギー社製:CY−205 100重量部と、HY−9
74J 23重量部の混合物)を50℃に加温し、35
4mlを15分で注入した。
Comparative Example 4 Using the same hollow fiber-shaped porous separation membrane as in Example 1, an element having an end sealing portion made of an epoxy resin was prepared in the following steps. The both ends of the 586 hollow fiber-shaped porous separation membranes are heat-sealed and sealed, and 3 to 5 cm of the ends are coated with a fluororesin surface modifier (manufactured by Junko Co., tetra-etch).
After the treatment, 100 parts by weight of an epoxy resin (manufactured by Ciba-Geigy: CY-205 and HY-9) are used instead of FEP.
74J 23 parts by weight) was heated to 50 ° C.
4 ml were injected in 15 minutes.

【0044】その後、75℃で3時間、さらに120℃
で2時間保持してエポキシ樹脂を硬化させた。受け皿を
はずして、外筒から出ているエポキシ樹脂部分を切断
し、封止剤がエポキシ樹脂である構造の中空糸状多孔質
分離膜エレメントを得た。得られた中空糸状多孔質分離
膜エレメントは、その末端封止部の樹脂に気泡は見られ
なかった。
Thereafter, at 75 ° C. for 3 hours, and further at 120 ° C.
For 2 hours to cure the epoxy resin. The tray was removed and the epoxy resin portion protruding from the outer cylinder was cut to obtain a hollow fiber-shaped porous separation membrane element having a structure in which the sealing agent was an epoxy resin. In the obtained hollow fiber-shaped porous separation membrane element, no bubbles were observed in the resin at the terminal sealing portion.

【0045】<物性の測定>実施例1〜2 実施例1〜2で得られた中空糸状多孔質分離膜エレメン
トを用いて、0.2kg/cm2でエアーリークテスト
を行なったが、エアーリークは認められず、末端封止が
完全に行なわれていることが確認できた。また、実施例
1〜2で得られた中空糸状多孔質分離膜エレメントを用
いて、膜間差圧4kg/cm2、400時間の条件で、
水、40%アンモニア水、10%塩酸、アセトン、トル
エン、ジエチルアミン、塩化メチレンの各濾過試験を行
なった後、再度エアリークテストを実施したところ、エ
アリークは認められなかった。
<Measurement of Physical Properties> Examples 1 and 2 An air leak test was performed at 0.2 kg / cm 2 using the hollow fiber-shaped porous separation membrane elements obtained in Examples 1 and 2. Was not recognized, and it was confirmed that the terminal sealing was completely performed. Further, using the hollow fiber-shaped porous separation membrane element obtained in Examples 1 and 2 , under the conditions of a transmembrane pressure difference of 4 kg / cm 2 and 400 hours,
After performing each filtration test of water, 40% ammonia water, 10% hydrochloric acid, acetone, toluene, diethylamine, and methylene chloride, an air leak test was performed again. As a result, no air leak was observed.

【0046】実施例1〜2で得られた中空糸状多孔質分
離膜エレメントについては、濃硫酸、20%カセイソー
ダ、10%硝酸に3ケ月漬浸後に、エアリークテストお
よび5kg/cm2耐圧試験を行ったが、エアリークは
認められなかった。
The hollow fiber-like porous separation membrane elements obtained in Examples 1 and 2 were immersed in concentrated sulfuric acid, 20% caustic soda, and 10% nitric acid for 3 months, and then subjected to an air leak test and a 5 kg / cm 2 pressure resistance test. However, no air leak was observed.

【0047】さらに、実施例1〜2で得られた中空糸状
多孔質分離膜エレメントを用いて、150℃、湿度10
0%で1時間加熱後、急速冷却し、4℃に1時間保持
後、再び150℃に加熱するヒートサイクルテストを1
ケ月行なった後、エアリークテストおよび5kg/cm
2耐圧試験を行ったところ、エアリークは認められなか
った。
Further, the hollow fiber-shaped porous separation membrane element obtained in Examples 1 and 2 was used at 150 ° C. and 10% humidity.
After heating at 0% for 1 hour, rapidly cooling, holding at 4 ° C. for 1 hour, and then heating again to 150 ° C., a heat cycle test was performed for 1 hour.
After 5 months, air leak test and 5kg / cm
2 When a pressure resistance test was performed, no air leak was observed.

【0048】比較例1〜3 これに対して、比較例1〜2で得られた中空糸状多孔質
分離膜エレメントを用いて、0.2kg/cm2でエア
リークテストを行なったところ、いずれにもエアリーク
が認められた。比較例3では、前記したとおり満足な末
端封止部が作製できなかったので、エアリークテストは
行なわなかった。
Comparative Examples 1 to 3 In contrast, an air leak test was performed at 0.2 kg / cm 2 using the hollow fiber-shaped porous separation membrane elements obtained in Comparative Examples 1 and 2. An air leak was observed. In Comparative Example 3, as described above, a satisfactory end sealing portion could not be produced, and thus no air leak test was performed.

【0049】比較例4 比較例4で得られた中空糸状多孔質分離膜エレメントを
用いて、0.2kg/cm2でエアリークテストを行な
ったところ、エアリークは認められなかった。しかしな
がら、膜間差圧4kg/cm2、400時間の条件で、
水、40%アンモニア水、10%塩酸、アセトン、トル
エン、ジエチルアミンおよび塩化メチレンの各濾過試験
を行なった後、再度エアリークテストを実施したとこ
ろ、40%アンモニア水、アセトン、ジエチルアミンお
よび塩化メチレンの濾過で末端封止部のクラックとエア
リークが認められた。特に、ジエチルアミンと塩化メチ
レンの濾過試験後には、末端封止部に多数のヒビ割れと
一部欠損が認められた。
Comparative Example 4 An air leak test was performed at 0.2 kg / cm 2 using the hollow fiber-shaped porous separation membrane element obtained in Comparative Example 4, and no air leak was observed. However, under the conditions of a transmembrane pressure difference of 4 kg / cm 2 and 400 hours,
After performing each filtration test of water, 40% ammonia water, 10% hydrochloric acid, acetone, toluene, diethylamine and methylene chloride, an air leak test was again performed. As a result, filtration of 40% ammonia water, acetone, diethylamine and methylene chloride was performed. Cracks and air leaks at the end sealing portion were observed. In particular, after the filtration test of diethylamine and methylene chloride, many cracks and partial defects were observed in the terminal sealing portion.

【0050】また、濃硫酸、20%カセイソーダおよび
10%硝酸に3ケ月漬浸後に、エアリークテストおよび
5kg/cm2耐圧試験を行ったところ、同様に末端封
止部のクラックとエアリークが認められた。さらに、ヒ
ートサイクルテストでは、一日以内に末端封止部が破壊
した。
After immersion in concentrated sulfuric acid, 20% caustic soda and 10% nitric acid for 3 months, an air leak test and a 5 kg / cm 2 pressure resistance test were carried out. . Further, in the heat cycle test, the end sealing portion was broken within one day.

【0051】[0051]

【発明の効果】本発明の製造方法による中空糸状多孔質
分離膜エレメントは、耐熱性、耐薬品性が改善され、末
端部の封止も完全であるため、酸性やアルカリ性溶液お
よび有機溶剤を溶媒または洗浄等に使用する場合、ある
いは蒸気滅菌等の滅菌・殺菌を必要とする分離膜モジュ
ールに好適である。
The hollow fiber porous separation membrane element according to the production method of the present invention has improved heat resistance and chemical resistance, and has a complete end seal, so that an acidic or alkaline solution or an organic solvent can be used as a solvent. It is suitable for use in washing or the like, or for a separation membrane module requiring sterilization or sterilization such as steam sterilization.

【0052】本発明の中空糸状多孔質分離膜エレメント
の製造方法は、末端封止部の微細成型性を大幅に改善し
たものである。そのために、封止剤として高粘度の熱溶
融性フッ素樹脂を使用しても、充填率の高い中空糸状多
孔質分離膜エレメントを得ることができる。
The method for producing a hollow fiber-shaped porous separation membrane element of the present invention greatly improves the fine moldability of the end sealing portion. Therefore, even if a high-viscosity heat-meltable fluororesin is used as a sealing agent, a hollow fiber-shaped porous separation membrane element with a high filling rate can be obtained.

【図面の簡単な説明】[Brief description of the drawings]

【図1】低充填率で中空糸状多孔質分離膜の末端封止部
を形成した予備成型物の一実施例を示す断面略図であ
る。
FIG. 1 is a schematic cross-sectional view showing one embodiment of a preform having a terminal filling portion of a hollow fiber-shaped porous separation membrane formed at a low filling rate.

【図2】予備成型物を加熱・加圧して所望の形状に成型
した末端封止部を示す断面略図である。
FIG. 2 is a schematic cross-sectional view showing a terminal sealing portion formed by heating and pressing a preform into a desired shape.

【図3】本発明の製造方法に使用する装置の一例を示し
た略図である。
FIG. 3 is a schematic view showing an example of an apparatus used in the manufacturing method of the present invention.

【図4】予備成型物を加圧するために、図3の装置の移
動部を移動させたことを示す略図である。
FIG. 4 is a schematic view showing that the moving part of the apparatus of FIG. 3 has been moved to pressurize the preform.

【図5】本発明の製造方法において、エレメントとして
仕上げる段階での外筒装着工程を示す略図である。
FIG. 5 is a schematic view showing an outer cylinder mounting step in a stage of finishing as an element in the manufacturing method of the present invention.

【図6】封止部の端末部を切断除去する工程を示す略図
である。
FIG. 6 is a schematic view showing a step of cutting and removing a terminal portion of a sealing portion.

【図7】封止部のステンレス棒を抜き取った後のエレメ
ントを示す略図である。
FIG. 7 is a schematic view showing the element after the stainless steel bar of the sealing portion is extracted.

【図8】本発明の製造方法により得られる中空糸状多孔
質分離膜エレメント端部断面の一例を示す略図である。
FIG. 8 is a schematic view showing an example of a cross section of an end portion of a hollow fiber-shaped porous separation membrane element obtained by the production method of the present invention.

【符号の説明】[Explanation of symbols]

1 ステンレス棒を挿入したPTFE多孔質チューブ 2 熱溶融性樹脂封止剤 3 移動部 4 予備成型物受け部 5 ステンレス製外筒 6 ステンレス棒 7 PTFE多孔質チューブ 1 PTFE porous tube with stainless steel rod inserted 2 Heat-meltable resin sealant 3 Moving part 4 Preformed product receiving part 5 Stainless steel outer cylinder 6 Stainless steel rod 7 PTFE porous tube

Claims (3)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 多数の中空糸状多孔質分離膜の一端を熱
溶融性樹脂中に挿入した形状の予備成型物を作成し、つ
いで該予備成型物の熱溶融性樹脂を加熱して溶融状態に
しながら周囲から加圧することにより、各中空糸状多孔
質分離膜相互の間隙を減少させて、所望形状の熱溶融性
樹脂からなる末端封止部を形成させることを特徴とする
中空糸状多孔質分離膜エレメントの製造方法。
1. A preform having a shape in which one end of a number of hollow fiber-like porous separation membranes is inserted into a hot-melt resin is prepared, and then the hot-melt resin of the preform is heated to a molten state. A hollow fiber-like porous separation membrane characterized in that the gap between the hollow fiber-like porous separation membranes is reduced by applying pressure from the surroundings to form a terminal sealing portion made of a heat-meltable resin in a desired shape. Element manufacturing method.
【請求項2】 予備成型物が中空糸状多孔質分離膜の一
端をこれが挿入できる穴を持つ熱溶融性樹脂成型物に挿
入したものを多数束ねたものであって、熱溶融性樹脂を
加熱溶融状態にしながら周囲から加圧することにより、
中空糸状多孔質分離膜を挿入した各熱溶融性樹脂成形物
を溶融一体化すると同時に各中空糸状多孔質分離膜相互
の間隙を減少させて、所望形状の熱溶融性樹脂からなる
末端封止部を形成させることを特徴とする請求項1記載
の中空糸状多孔質分離膜エレメントの製造方法。
2. A pre-molded product obtained by bundling a large number of hollow fiber-shaped porous separation membranes each having one end inserted into a hot-melt resin molded product having a hole into which the hollow fiber-shaped porous separation membrane can be inserted. By applying pressure from the surroundings while in a state,
Each of the heat-fusible resin molded products into which the hollow fiber-shaped porous separation membranes are inserted is melt-integrated, and at the same time, the gap between the hollow fiber-shaped porous separation membranes is reduced to form a terminal sealing portion made of a heat-meltable resin having a desired shape. The method for producing a hollow fiber-shaped porous separation membrane element according to claim 1, wherein
【請求項3】 予備成型物が中空糸状多孔質分離膜の一
端をこれが挿入できる穴を多数持つ熱溶融性樹脂成型物
に多数挿入したものであって、熱溶融性樹脂を加熱溶融
状態にしながら周囲から加圧することにより、各中空糸
状多孔質分離膜相互の間隙を減少させて、所望形状の熱
溶融性樹脂からなる末端封止部を形成させることを特徴
とする請求項1記載の中空糸状多孔質分離膜エレメント
の製造方法。
3. The pre-molded product is obtained by inserting one end of a hollow fiber-shaped porous separation membrane into a hot-melt resin molded product having a large number of holes into which the hollow fiber-shaped porous separation membrane can be inserted. 2. The hollow fiber according to claim 1, wherein the pressure is applied from the periphery to reduce the gap between the hollow fiber porous separation membranes, thereby forming a terminal sealing portion made of a heat-meltable resin having a desired shape. A method for producing a porous separation membrane element.
JP3246584A 1991-08-30 1991-08-30 Method for producing hollow fiber-shaped porous separation membrane element Expired - Lifetime JP2993217B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3246584A JP2993217B2 (en) 1991-08-30 1991-08-30 Method for producing hollow fiber-shaped porous separation membrane element

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3246584A JP2993217B2 (en) 1991-08-30 1991-08-30 Method for producing hollow fiber-shaped porous separation membrane element

Publications (2)

Publication Number Publication Date
JPH0557153A JPH0557153A (en) 1993-03-09
JP2993217B2 true JP2993217B2 (en) 1999-12-20

Family

ID=17150592

Family Applications (1)

Application Number Title Priority Date Filing Date
JP3246584A Expired - Lifetime JP2993217B2 (en) 1991-08-30 1991-08-30 Method for producing hollow fiber-shaped porous separation membrane element

Country Status (1)

Country Link
JP (1) JP2993217B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7309424B2 (en) 2001-01-31 2007-12-18 Kabushiki Kaisha Toshiba Filtering apparatus, back wash method therefor, filtering device and power plant

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7309424B2 (en) 2001-01-31 2007-12-18 Kabushiki Kaisha Toshiba Filtering apparatus, back wash method therefor, filtering device and power plant
US7754074B2 (en) 2001-01-31 2010-07-13 Kabushiki Kaisha Toshiba Filtering apparatus, back wash method therefor, filtering device and power plant

Also Published As

Publication number Publication date
JPH0557153A (en) 1993-03-09

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