JPH089668B2 - Hydrophilized film and method for producing the same - Google Patents

Hydrophilized film and method for producing the same

Info

Publication number
JPH089668B2
JPH089668B2 JP61243372A JP24337286A JPH089668B2 JP H089668 B2 JPH089668 B2 JP H089668B2 JP 61243372 A JP61243372 A JP 61243372A JP 24337286 A JP24337286 A JP 24337286A JP H089668 B2 JPH089668 B2 JP H089668B2
Authority
JP
Japan
Prior art keywords
membrane
water
polysulfone
polyvinylpyrrolidone
hollow fiber
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
JP61243372A
Other languages
Japanese (ja)
Other versions
JPS6397634A (en
Inventor
良忠 酒井
昌明 島垣
和実 田中
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.)
Toray Industries Inc
Original Assignee
Toray Industries Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Toray Industries Inc filed Critical Toray Industries Inc
Priority to JP61243372A priority Critical patent/JPH089668B2/en
Publication of JPS6397634A publication Critical patent/JPS6397634A/en
Publication of JPH089668B2 publication Critical patent/JPH089668B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0081—After-treatment of organic or inorganic membranes
    • B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0081—After-treatment of organic or inorganic membranes
    • B01D67/009—After-treatment of organic or inorganic membranes with wave-energy, particle-radiation or plasma

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Plasma & Fusion (AREA)
  • Physics & Mathematics (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • External Artificial Organs (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)

Description

【発明の詳細な説明】 ［産業上の利用分野］ 本発明は、新規な親水化膜およびその製造法に関す
る。TECHNICAL FIELD The present invention relates to a novel hydrophilized film and a method for producing the same.

［従来の技術］ 従来、過処理や透析処理で用いられる水処理用膜
は、グリセリンなどの水溶性膜透過能維持剤を用いた
状態、膜素材として親水性高分子を用いた状態、水
を共存させた状態、などで供給されてきた。しかし、
では使用に先立って膜透過能維持剤を洗浄除去する必要
があり、即時使用ができないこと、では一般にポアサ
イズが小さくなり、分子量数万以上の成分の分離に使え
る膜ができにくいこと、では被処理液体が血液である
場合など、共存している水を予め被処理液体に変質を与
えない液体に置換する必要がある用途があり、即時使用
できないことなど、それぞれに問題がある。[Prior Art] Conventionally, water treatment membranes used in overtreatment or dialysis treatment have a water-soluble membrane permeability-maintaining agent such as glycerin, a hydrophilic polymer as a membrane material, or water. It has been supplied in a coexisting state. But,
Since it is necessary to wash and remove the membrane permeability maintaining agent prior to use, it is not possible to use immediately, then the pore size is generally small, and it is difficult to form a membrane that can be used to separate components with a molecular weight of tens of thousands or more. For example, when the liquid is blood, there is a use in which coexisting water needs to be replaced with a liquid that does not deteriorate the liquid to be treated in advance, and there are problems in that it cannot be used immediately.

一方、膜素材として、ポリエチレン、ポリプロピレ
ン、ポリマーボネート、ポリアクリロニトリル、ポリス
ルホン、ポリエステル、ポリ２弗化ビニリデン、ポリ４
弗化エチレン、ポリメチルメタクリレート、セルロース
トリアセテートなどの疎水性高分子を主たる素材とした
膜が過膜や透析膜として提供されているが、これらの
疎水性膜ではやの状態にしておかないと直ちには本
来の透過能を発揮できず、したがって前記のように即時
使用できない問題は疎水性膜の宿命とされてきた。ま
た、疎水性膜に対して親水性成分を導入し、固着させる
ことで即時使用を可能にするという例（例えば、特開昭
61−120602、特開昭61−125405、特開昭61−125408、特
開昭61−125409、特開昭61−133102、特開昭61−133105
など）もみられるが、これらでは親水性高分子の固着が
不充分で、使用中に膜から親水性成分が溶出してくるな
どの問題がある。On the other hand, as film materials, polyethylene, polypropylene, polymer bonates, polyacrylonitrile, polysulfones, polyesters, polyvinylidene difluoride, poly 4
Membranes composed mainly of hydrophobic polymers such as ethylene fluoride, polymethylmethacrylate, and cellulose triacetate are provided as permembranes and dialysis membranes. Has not been able to exert its original permeability, and thus the problem that it cannot be used immediately as described above has been destined for the hydrophobic membrane. In addition, an example in which a hydrophilic component is introduced into a hydrophobic film and fixed to the hydrophobic film to enable immediate use (see, for example, JP-A-
61-120602, JP-A-61-125405, JP-A-61-125408, JP-A-61-125409, JP-A-61-133102, JP-A-61-133105.
Etc.) are also observed, but there is a problem that the hydrophilic polymer is insufficiently fixed and the hydrophilic component is eluted from the membrane during use.

［発明が解決しようとする問題点］ 本発明者らは、かかる状況に鑑み、溶出性成分を伴わ
ずに疎水性膜を即時使えるようにするには如何にすべき
かにつき鋭意検討を重ねたところ本発明に到達した。[Problems to be Solved by the Invention] In view of the above situation, the present inventors have made earnest studies on how to immediately use a hydrophobic membrane without an elutable component. The present invention has been reached.

［問題点を解決するための手段］ 即ち、ポリスルホンを主たる素材とした疎水性膜へ、
該膜の製造行程中で放射線または／および熱により水不
溶化するポリビニルピロリドンを導入することにより、
溶出性成分を伴わずにポリスルホン膜を即時使えるよう
にしうることを見出した。[Means for Solving Problems] That is, to a hydrophobic membrane using polysulfone as a main material,
By introducing polyvinylpyrrolidone which is water-insoluble by radiation or / and heat in the production process of the membrane,
It has been found that the polysulfone membrane can be made ready for use without elutable components.

本発明のポリスルホンを主体とした疎水性成分として
は、ポリスルホンおよびその誘導体、あるいはポリスル
ホンを主体とするが共重合成分として親水性成分を少量
含む重合体などが用いられ、本手段は平衡吸水率（20
℃、相対湿度65％の雰囲気下に１週間置いて測定した吸
水率で、水重量／ポリマー重量を％で表示した値）が５
％以下、さらに望ましくは２％以下の素材に適用でき
る。As the hydrophobic component mainly composed of polysulfone of the present invention, polysulfone and a derivative thereof, or a polymer mainly composed of polysulfone but containing a small amount of a hydrophilic component as a copolymerization component is used. 20
Water absorption measured by leaving it in an atmosphere of ℃ and relative humidity of 65% for 1 week, and the value (% water weight / polymer weight) is 5
% Or less, more preferably 2% or less.

ポリビニルピロリドンの水不溶化手段として、放射線
を照射する方法と加熱する方法とがあるが、ポリスルホ
ンは、耐放射線性および耐熱性に共に優れた素材である
ので、両手段を併用することも可能である。As a water insolubilizing means for polyvinylpyrrolidone, there are a method of irradiating with radiation and a method of heating, but since polysulfone is a material excellent in both radiation resistance and heat resistance, it is possible to use both means in combination. .

放射線または／および熱により水不溶化する成分とし
て、ビニルピロリドンが用いられるが、その誘導体モノ
マー、さらには、オリゴマ、ポリマー等であってもよ
く、本発明でいう製造行程中で導入するビニルピロリド
ンには、これらポリマー等も含まれる。Vinylpyrrolidone is used as a component which becomes insoluble in water by radiation and / or heat, but its derivative monomer, further, an oligomer, a polymer or the like may be used, and vinylpyrrolidone introduced in the production process in the present invention is , These polymers and the like are also included.

水不溶化手段としての放射線としては、ガンマー線、
紫外線、電子線などが用いられるが、特にガンマー線で
は浸透性が高いので単一膜だけでなく、膜集合体や膜を
組込んだモジュール状態でもポリビニルピロリドンの水
不溶化処理が行なえるので好適に用いられる。水不溶化
手段としての加熱手段としては、乾熱、湿熱、温浴加熱
のいずれも用いることができる。加熱温度としては、ポ
リスルホンの軟化点や融点、ポリビニルピロリドンの熱
分解温度などを考慮する必要があるが、50℃ないし200
℃が好ましい。また、加熱処理をポリビニルピロリドン
を水不溶化する手段としてだけでなく、ポアサイズの調
整手段も兼ね合せた手段として用いることも可能であ
る。Radiation as water insolubilization means, gamma rays,
Ultraviolet rays, electron beams, etc. are used, but especially since gamma rays have high permeability, it is possible to perform water insolubilization treatment of polyvinylpyrrolidone not only in a single membrane but also in a membrane assembly or a module state in which a membrane is incorporated. Used. As the heating means as the water insolubilizing means, any of dry heat, wet heat and hot bath heating can be used. As the heating temperature, it is necessary to consider the softening point and melting point of polysulfone, the thermal decomposition temperature of polyvinylpyrrolidone, etc.
C is preferred. Further, the heat treatment can be used not only as a means for making polyvinylpyrrolidone insoluble in water but also as a means that also serves as a means for adjusting the pore size.

ポリビニルピロリドンを導入する製膜段階としては、
膜素材へのブロック共重合体化、製膜原液への混入、ポ
リスルホン膜製膜後の後処理など、いずれの段階でも良
いが、製膜原液への混入や後処理による導入が大きな孔
を確保しやすいという点、ポリビニルピロリドンの使用
量を削減できるという点などで有利である。また、放射
線照射や加熱処理を膜や膜を組込んだモジュールの殺菌
手段を兼ねたものとすることも可能である。As a film forming step of introducing polyvinylpyrrolidone,
Any step may be performed, such as block copolymerization into the membrane material, incorporation into the membrane-forming stock solution, and post-treatment after polysulfone membrane formation, but large holes are ensured by incorporation into the membrane-forming stock solution or introduction by post-treatment. It is advantageous in that it is easy to do and that the amount of polyvinylpyrrolidone used can be reduced. Further, the irradiation of radiation and the heat treatment may also serve as a sterilizing means for the membrane or the module incorporating the membrane.

本発明でいう膜の形態は特に限定するものではなく、
例えばシート状、中空糸状、マイクロカプセル状の膜な
どが挙げられる。The form of the film in the present invention is not particularly limited,
Examples thereof include sheet-shaped, hollow fiber-shaped, and microcapsule-shaped membranes.

以下、本発明の有効性を実施例をもって説明する。そ
こで用いた測定法は次の通りである。Hereinafter, the effectiveness of the present invention will be described with reference to examples. The measuring method used there is as follows.

（１） 透水性 中空糸膜の場合は、両端に還流液溶の孔を備えたガラ
ス製のケースに該中空糸膜を挿入し、市販のポッティン
グ剤を用いて小型モジュールを作製し、37℃に保って中
空糸内側に水圧をかけ膜を通して外側へ透過する一定時
間の水の量と有効膜面積および膜間圧力差から算出する
方法で透水性能を測定した。(1) Water-permeable In the case of a hollow fiber membrane, the hollow fiber membrane is inserted into a glass case having holes for reflux liquid dissolution at both ends, and a small module is prepared using a commercially available potting agent, and the temperature is 37 ° C. The water permeation performance was measured by a method in which water pressure was applied to the inside of the hollow fiber and the water was permeated to the outside through the membrane for a certain period of time, and was calculated from the effective membrane area and the transmembrane pressure difference.

平膜の場合は、撹拌円筒セルを用いて同様にして測定
した。In the case of a flat membrane, the same measurement was performed using a stirring cylindrical cell.

（２） 溶出物 膜0.5gを70℃温水50ccで１時間加熱して試験液を調製
する。試験液の波長220〜350μｍにおける吸光度を測定
する。なお、透析型人工腎臓装置承認基準では、本条件
での規格を0.1以下としている。(2) Eluate A test solution is prepared by heating 0.5 g of the membrane with 50 cc of hot water at 70 ° C for 1 hour. The absorbance of the test solution at a wavelength of 220 to 350 μm is measured. The dialysis-type artificial kidney device approval standard sets the standard under this condition to 0.1 or less.

［実施例］ 実施例１ ポリスルホン（ユーデルポリサルホンＰ−3500）15
部、ポリビニルビロリドン（Ｋ−90）８部、ジメチルア
セトアミド75部、水２部からなる原液から製膜した中空
糸膜を185℃、1.5時間乾熱処理し、ポリビニルビロリド
ンの水不溶化処理を施した。この完全ドライ膜の透水性
を測定したところ15000の値を得た。この膜の表面には
0.2μｍ程度の孔があり、常圧で水漏れ性の良いことか
ら、浄水器用として利用できる。[Example] Example 1 Polysulfone (Udel Polysulfone P-3500) 15
Part, polyvinylpyrrolidone (K-90) 8 parts, dimethylacetamide 75 parts, and a hollow fiber membrane formed from an undiluted solution of water 2 parts by water are heat-treated at 185 ° C for 1.5 hours to make polyvinylpyrrolidone insoluble in water. Was applied. When the water permeability of this completely dry film was measured, a value of 15000 was obtained. On the surface of this membrane
Since it has a hole of about 0.2 μm and has good water leakage at normal pressure, it can be used as a water purifier.

実施例２ 実施例１と同様にして製膜した中空糸膜を170℃、５
時間乾燥処理し、親水化膜を作った。本中空糸膜を膜面
積0.15m2になるように束ね、モジュール化後、2.5Mrad
γ線照射処理後乾燥し、ドライ膜として牛血（ヘマトク
リット値40％、総タンパク濃度65g/dl）での血漿分離性
能を測定したところ、温度37℃、膜間圧力差47mmHg、血
液流量50ml/minで血漿過流量16ml/minの性能を得た。
水がついていないため、初期からタンパク透過率（液
中濃度／血液中濃度）が95％を越える優れたドライ採血
漿膜としての性能を認めた。Example 2 A hollow fiber membrane produced in the same manner as in Example 1 was heated at 170 ° C. for 5
It was dried for an hour to form a hydrophilic film. This hollow fiber membrane was bundled so that the membrane area was 0.15 m 2 , and after modularization, 2.5 Mrad
After γ-irradiation treatment, it was dried and the plasma separation performance was measured using bovine blood (hematocrit value 40%, total protein concentration 65g / dl) as a dry membrane. Temperature 37 ° C, transmembrane pressure difference 47mmHg, blood flow 50ml / A plasma overflow of 16 ml / min was obtained at min.
Since there was no water, the performance as an excellent dry plasma membrane with protein permeability (concentration in liquid / concentration in blood) exceeding 95% was recognized from the initial stage.

実施例３ 実施例１と同様にして製膜した中空糸膜をモジュール
化後、水を充填させ、2.5Mradγ線照射による後処理を
施した。この膜を乾燥後、透水性能を測定したところ11
000の性能を得た。Example 3 A hollow fiber membrane produced in the same manner as in Example 1 was modularized, filled with water, and post-treated with 2.5 Mrad γ-ray irradiation. After the membrane was dried, the water permeability was measured to be 11
Got 000 performance.

実施例４ 実施例１〜３の中空糸膜の溶出物試験をしたところ、
すべて220nm〜350nmでの吸光度は0.1以下であった。Example 4 When the hollow fiber membranes of Examples 1 to 3 were subjected to an eluate test,
All the absorbances at 220 nm to 350 nm were less than 0.1.

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ０８Ｊ 7/00 ３０５ 7/04 ＣＥＺ Ｔ // Ｃ０８Ｌ 81:06 (56)参考文献 特開 昭56−38333（ＪＰ，Ａ) 特開 昭56−157437（ＪＰ，Ａ) 特開 昭53−134876（ＪＰ，Ａ) 特開 昭63−51129（ＪＰ，Ａ) 特公 昭56−2094（ＪＰ，Ｂ２)─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification number Office reference number FI Technical display location C08J 7/00 305 7/04 CEZ T // C08L 81:06 (56) References JP-A-56 -38333 (JP, A) JP-A-56-157437 (JP, A) JP-A-53-134876 (JP, A) JP-A-63-51129 (JP, A) JP-B-56-2094 (JP, B2) )

Claims (3)

【特許請求の範囲】[Claims] 【請求項１】ポリスルホンを主体とした疎水性成分と、
物理的に不溶化したポリビニルピロリドンとからなる親
水化膜。1. A hydrophobic component composed mainly of polysulfone,
A hydrophilic film made of polyvinylpyrrolidone physically insolubilized. 【請求項２】親水化膜が、中空糸膜であることを特徴と
する請求項１記載の親水化膜。2. The hydrophilic membrane according to claim 1, wherein the hydrophilic membrane is a hollow fiber membrane. 【請求項３】ポリスルホンを主体とした疎水性高分子を
主たる素材とした膜の製造工程中でビニルピロリドンを
導入し該ビニルピロリドンを放射線または／および熱に
より水不溶化することを特徴とする親水化膜の製造方
法。3. A hydrophilization characterized in that vinylpyrrolidone is introduced in a process of manufacturing a membrane mainly composed of a hydrophobic polymer mainly composed of polysulfone to make the vinylpyrrolidone water-insoluble by radiation and / or heat. Membrane manufacturing method.
JP61243372A 1986-10-14 1986-10-14 Hydrophilized film and method for producing the same Expired - Lifetime JPH089668B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP61243372A JPH089668B2 (en) 1986-10-14 1986-10-14 Hydrophilized film and method for producing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61243372A JPH089668B2 (en) 1986-10-14 1986-10-14 Hydrophilized film and method for producing the same

Related Child Applications (3)

Application Number Title Priority Date Filing Date
JP7159451A Division JPH0852471A (en) 1995-06-26 1995-06-26 Water purifier and its production
JP7159452A Division JPH0852331A (en) 1995-06-26 1995-06-26 Plasma collecting membrane and production thereof
JP09110911A Division JP3132415B2 (en) 1997-04-28 1997-04-28 Hydrophilic dialysis membrane

Publications (2)

Publication Number Publication Date
JPS6397634A JPS6397634A (en) 1988-04-28
JPH089668B2 true JPH089668B2 (en) 1996-01-31

Family

ID=17102866

Family Applications (1)

Application Number Title Priority Date Filing Date
JP61243372A Expired - Lifetime JPH089668B2 (en) 1986-10-14 1986-10-14 Hydrophilized film and method for producing the same

Country Status (1)

Country Link
JP (1) JPH089668B2 (en)

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