JP2018158275A - Hollow fiber membrane for endotoxin capture filter - Google Patents

Hollow fiber membrane for endotoxin capture filter Download PDF

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JP2018158275A
JP2018158275A JP2017055304A JP2017055304A JP2018158275A JP 2018158275 A JP2018158275 A JP 2018158275A JP 2017055304 A JP2017055304 A JP 2017055304A JP 2017055304 A JP2017055304 A JP 2017055304A JP 2018158275 A JP2018158275 A JP 2018158275A
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hollow fiber
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endotoxin
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JP7224750B2 (en
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中塚　修志
Nobuyuki Nakatsuka
修志 中塚
智一 綿部
Tomokazu Watabe
智一 綿部
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Daicen Membrane Systems Ltd
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Abstract

PROBLEM TO BE SOLVED: To provide a hollow fiber membrane having good water permeable performance and endotoxin capture performance.SOLUTION: A hollow fiber membrane for high water permeable endotoxin capture filter contains polyether sulfone that is 80 mass% or more of a hollow fiber membrane component, and has macrovoid having a maximum diameter of 10 μm or more in a cross section of the hollow fiber membrane, where an area ratio of the macrovoid to a cross-sectional area of the hollow fiber membrane is 20-40%, pure water permeation coefficient (PWP) is 1600 L/mh(0.1 MPa) or more, and endotoxin blocking performance (ET LRV) measured with the use of a test liquid having an endotoxin concentration of 100 EU/ml according to JIS K 3824 is 3 or more.SELECTED DRAWING: None

Description

本発明は、処理対象となる原水中に含まれているエンドトキシンを捕捉するためのエンドトキシン捕捉フィルター用中空糸膜に関する。   The present invention relates to a hollow fiber membrane for an endotoxin capturing filter for capturing endotoxin contained in raw water to be treated.

人工透析用水や注射用水などの医療用精製水には、エンドトキシンが含まれていないことが要求されるほか、人工腎臓などの人工臓器もエンドトキシンの透過を抑制できることが要求されている。   Medical purified water such as artificial dialysis water and injection water is required not to contain endotoxin, and an artificial organ such as an artificial kidney is required to be able to suppress permeation of endotoxin.

特許文献１には、高い透水性とエンドトキシン除去性能を有している、ポリスルホン系ポリマーなどの疎水性高分子よりなる透析液清浄化用中空糸膜の発明が記載されている。
特許文献２には、エンドトキシンやアルブミンの透過率が小さいポリスルホン系中空糸型人工腎臓とその製造方法の発明が記載されている。 Patent Document 1 describes an invention of a dialysis fluid cleaning hollow fiber membrane made of a hydrophobic polymer such as a polysulfone polymer having high water permeability and endotoxin removal performance.
Patent Document 2 describes an invention of a polysulfone-based hollow fiber artificial kidney having a low permeability of endotoxin and albumin and a method for producing the same.

特開２００４−１２１６０８号公報JP 2004-121608 A 特開平１１−１０４２３５号公報Japanese Patent Laid-Open No. 11-104235

本発明は、透水性能とエンドトキシン阻止性能の両方が高いエンドトキシン捕捉フィルター用中空糸膜を提供することを課題とする。   An object of the present invention is to provide a hollow fiber membrane for an endotoxin-capturing filter having high water permeability and endotoxin blocking performance.

本発明は、中空糸膜成分中の８０質量％以上がポリエーテルスルホンであり、
中空糸膜断面に最大径が１０μｍ以上のマクロボイドを有し、前記マクロボイドの中空糸膜断面積に占める面積割合が２０〜４０％であり、
純水透過係数（ＰＷＰ）が１６００L／m2・h(0.1MPa)以上で、エンドトキシン濃度が１００ＥＵ/ｍｌの試験液を用い、JIS K3824に準じて測定されたエンドトキシン阻止性能（ＥＴ ＬＲＶ）が３以上である、エンドトキシン捕捉フィルター用中空糸膜を提供する。 In the present invention, 80% by mass or more of the hollow fiber membrane component is polyethersulfone,
The cross section of the hollow fiber membrane has a macro void having a maximum diameter of 10 μm or more, and the area ratio of the macro void to the cross section of the hollow fiber membrane is 20 to 40%.
The endotoxin blocking performance (ET LRV) measured according to JIS K3824 using a test solution with a pure water permeability coefficient (PWP) of 1600 L / m 2 · h (0.1 MPa) or more and an endotoxin concentration of 100 EU / ml is 3 A hollow fiber membrane for an endotoxin-capturing filter as described above is provided.

本発明のエンドトキシン捕捉フィルター用中空糸膜は、透水性能とエンドトキシン阻止性能が優れている。   The hollow fiber membrane for an endotoxin capture filter of the present invention is excellent in water permeability and endotoxin blocking performance.

実施例１で得られた中空糸膜の断面のＳＥＭ写真。2 is an SEM photograph of a cross section of the hollow fiber membrane obtained in Example 1. FIG. 比較例１で得られた中空糸膜の断面のＳＥＭ写真。3 is an SEM photograph of a cross section of the hollow fiber membrane obtained in Comparative Example 1. FIG.

＜エンドトキシン捕捉フィルター用中空糸膜＞
本発明のエンドトキシン捕捉フィルター用中空糸膜（以下、「本発明の中空糸膜」という）は、中空糸膜を構成する成分中の８０質量％以上がポリエーテルスルホンからなるものであり、より好ましくは１００質量％がポリエーテルスルホンからなるものである。
８０質量％〜１００質量％未満がポリエーテルスルホンであるときの残部のポリマー成分は、ポリアクリロニトリル、ポリメチルメタクリレートなどから選ばれるものが好ましい。 <Hollow fiber membrane for endotoxin capture filter>
The hollow fiber membrane for endotoxin-capturing filter of the present invention (hereinafter referred to as “the hollow fiber membrane of the present invention”) is more preferably 80% by mass or more of the components constituting the hollow fiber membrane, which is composed of polyethersulfone. 100% by mass consists of polyethersulfone.
The remaining polymer component when 80% by mass to less than 100% by mass is polyethersulfone is preferably selected from polyacrylonitrile, polymethyl methacrylate and the like.

本発明の中空糸膜の内径および外径は特に制限されるものではなく、外径は２５０〜６００μmが好ましく、３００〜５５０μmがより好ましく、内径は２００〜４５０μmが好ましく、２００〜４００μmがより好ましい。   The inner diameter and outer diameter of the hollow fiber membrane of the present invention are not particularly limited, and the outer diameter is preferably 250 to 600 μm, more preferably 300 to 550 μm, and the inner diameter is preferably 200 to 450 μm, more preferably 200 to 400 μm. .

本発明の中空糸膜は、膜断面（半径方向の断面）に最大径が１０μm以上のマクロボイドの中空糸膜断面積に占める面積割合は２０〜４０％である。前記マクロボイドの占有面積が４０％を超えると透水性能が低下する。   The hollow fiber membrane of the present invention has an area ratio of 20 to 40% in the cross-sectional area of a macrovoid having a maximum diameter of 10 μm or more in the membrane cross section (radial cross section). When the occupied area of the macro voids exceeds 40%, the water permeability is deteriorated.

本発明の中空糸膜は、純水透過係数（ＰＷＰ）が１６００L／m2・h(0.1MPa)以上である。
本発明の中空糸膜は、エンドトキシン濃度が１００ＥＵ/ｍｌの試験液を用い、JIS K3824に準じて測定されたエンドトキシン阻止性能（ＥＴ ＬＲＶ）は３以上であり、好ましくは４以上である。 The hollow fiber membrane of the present invention has a pure water permeability coefficient (PWP) of 1600 L / m 2 · h (0.1 MPa) or more.
The hollow fiber membrane of the present invention has an endotoxin inhibition performance (ET LRV) measured according to JIS K3824 using a test solution having an endotoxin concentration of 100 EU / ml, preferably 4 or more.

＜本発明の中空糸膜の製造方法＞
本発明の中空糸膜の製造方法は、公知の紡糸工程を含んでいる。
紡糸工程で実施する紡糸法としては、公知の乾湿式紡糸法、乾式紡糸法、湿式紡糸法などを使用することができるが、乾湿式紡糸法、湿式紡糸法が好ましい。 <Method for producing hollow fiber membrane of the present invention>
The method for producing a hollow fiber membrane of the present invention includes a known spinning process.
As the spinning method carried out in the spinning step, known dry and wet spinning methods, dry spinning methods and wet spinning methods can be used, but dry and wet spinning methods and wet spinning methods are preferred.

製膜成分は、ポリエーテルスルホン(PES)が８０質量％以上であり、他はポリアクリロニトリル、ポリメチルメタクリレートなどを使用することができるが、１００質量％がポリエーテルスルホンであることが好ましい。   As the film forming component, polyethersulfone (PES) is 80% by mass or more, and polyacrylonitrile, polymethylmethacrylate, and the like can be used for others, but 100% by mass is preferably polyethersulfone.

溶媒は、ジメチルスルホキシド、ジメチルホルムアミド、ジメチルアセトアミド、Ｎ−メチルピロリドンから選ばれるものを挙げることができ、これらの中でもジメチルスルホキシド(DMSO)が好ましい。   Examples of the solvent include those selected from dimethyl sulfoxide, dimethylformamide, dimethylacetamide, and N-methylpyrrolidone, and among these, dimethyl sulfoxide (DMSO) is preferable.

非溶媒は、ポリエチレングリコール、ポリプロピレングリコール、ポリビニルピロリドンなどを挙げることができるが、ポリエチレングリコールが好ましい。   Examples of the non-solvent include polyethylene glycol, polypropylene glycol, and polyvinyl pyrrolidone, but polyethylene glycol is preferable.

製膜溶液組成物中の製膜成分（ポリマー成分）の濃度は１０〜３０質量％が好ましい。
紡糸するときの製膜溶液組成物の温度は４０〜６０℃が好ましい。
ノズルから紡糸するときは、内部凝固液として水、ポリエチレングリコールおよびジメチルスルホキシドの混合溶液を使用することが好ましい。
前記内部凝固液は、水１５〜２５質量％、ポリエチレングリコール１５〜２５質量％およびジメチルスルホキシド５０〜７０質量％からなるものが好ましい。
内部凝固液の温度は、製膜溶液組成物の温度と同程度か低い温度であることが好ましい。 The concentration of the film-forming component (polymer component) in the film-forming solution composition is preferably 10 to 30% by mass.
The temperature of the film-forming solution composition when spinning is preferably 40 to 60 ° C.
When spinning from a nozzle, it is preferable to use a mixed solution of water, polyethylene glycol and dimethyl sulfoxide as the internal coagulation liquid.
The internal coagulating liquid is preferably composed of 15 to 25% by mass of water, 15 to 25% by mass of polyethylene glycol and 50 to 70% by mass of dimethyl sulfoxide.
The temperature of the internal coagulation liquid is preferably the same as or lower than the temperature of the film forming solution composition.

乾湿式紡糸を適用するときは、紡糸後、空気中を走行させ、外部凝固液中に導入して凝固させた後、水洗し、乾燥させる。
湿式紡糸法を適用するときは、紡糸後、外部凝固液中に導入して凝固させた後、水洗し、乾燥させる。 When dry-wet spinning is applied, it is run in the air after spinning, introduced into an external coagulation liquid, solidified, washed with water and dried.
When the wet spinning method is applied, after spinning, it is introduced into an external coagulation liquid and coagulated, then washed with water and dried.

（１）膜構造（中空糸内表面、外表面、断面の観察方法）
中空糸膜を切断し、断面の走査型電子顕微鏡（SEM） 写真を倍率200〜300倍で撮影した。中空糸膜の断面画像を得た後、前記断面画像から断面積に占めるボイドの面積を計測した。 (1) Membrane structure (hollow fiber inner surface, outer surface, cross-section observation method)
The hollow fiber membrane was cut and a cross-sectional scanning electron microscope (SEM) photograph was taken at a magnification of 200 to 300 times. After obtaining the cross-sectional image of the hollow fiber membrane, the area of voids in the cross-sectional area was measured from the cross-sectional image.

（２）分画分子量
分子量の異なる各種蛋白質（γグロブリン、コンアルブミン、トリプシン）を標準溶質として膜ろ過を行い、それぞれの排除率を測定して、分子量と排除率の関係をグラフにプロットし、得られた分子量排除率曲線より、排除率９０％ に相当する分子量を求めた。 (2) Fractionated molecular weight Various proteins (γ globulin, conalbumin, trypsin) with different molecular weights were subjected to membrane filtration as standard solutes, the respective exclusion rates were measured, and the relationship between the molecular weight and the exclusion rate was plotted in a graph. From the obtained molecular weight exclusion rate curve, a molecular weight corresponding to an exclusion rate of 90% was determined.

（３）伸縮率
実施例および比較例で得た中空糸膜の各１０本を３０ｃｍに切断し、９０℃の恒温水槽中に２時間浸漬させた後、糸長を測定し伸縮率を算出した。 (3) Stretch rate Ten hollow fiber membranes obtained in Examples and Comparative Examples were each cut into 30 cm and immersed in a constant temperature water bath at 90 ° C. for 2 hours, and then the yarn length was measured to calculate the stretch rate. .

（４）純水透過係数（PWP）
実施例および比較例で得た中空糸膜を純水に２時間浸漬した後、中空糸の一端側を閉じた状態で、他端側から純水を０．１ＭＰａで供給し、中空糸膜から一定時間に透過する純水の容量を測定した。この容量を採取時間（ｈ）、中空糸膜内表面の膜面積（ｍ2）で除して、純水透過係数〔Ｌ／ｍ2・ｈ（０．１ＭＰａ）〕を求めた。 (4) Pure water permeability coefficient (PWP)
After immersing the hollow fiber membranes obtained in Examples and Comparative Examples in pure water for 2 hours, with one end side of the hollow fiber closed, pure water was supplied at 0.1 MPa from the other end side, from the hollow fiber membrane The volume of pure water that permeates for a certain time was measured. This volume was divided by the sampling time (h) and the membrane area (m 2 ) on the inner surface of the hollow fiber membrane to obtain a pure water permeability coefficient [L / m 2 · h (0.1 MPa)].

（５）エンドトキシン阻止性能（ET LRV）
中空糸膜を２液硬化型ウレタン接着剤で、ケースハウジングに接着させ、エンドトキシン濃度が１万ＥＵ/ｍｌの試験液を用い、JIS K3824に準じてエンドトキシン阻止性能を測定した。 (5) Endotoxin blocking performance (ET LRV)
The hollow fiber membrane was adhered to the case housing with a two-component curable urethane adhesive, and the endotoxin blocking performance was measured according to JIS K3824 using a test solution having an endotoxin concentration of 10,000 EU / ml.

実施例１、２および比較例１
＜製膜溶液組成物＞
表１に示すジメチルスルホキシド（DMSO）、ポリエチレングリコール（PEG；MW 200）に対して、ポリエーテルスルホン（住友ケムテック社製スミカエクセル5200P）（PES）を加え、８０℃で約８時間加熱して溶解し、製膜溶液組成物を得た。 Examples 1 and 2 and Comparative Example 1
<Film forming solution composition>
Polyethersulfone (Sumitomo Chemtec 5200P manufactured by Sumitomo Chemtech) (PES) is added to dimethyl sulfoxide (DMSO) and polyethylene glycol (PEG; MW 200) shown in Table 1, and dissolved by heating at 80 ° C. for about 8 hours Thus, a film forming solution composition was obtained.

＜中空糸型半透膜の製造＞
上記の製膜溶液組成物を８０℃で１５時間静置し脱泡した。
脱泡した製膜溶液組成物を用い、５０℃に加温した二重紡糸ノズルより押し出し紡糸した。表１に示す内部凝固液を使用した。
二重紡糸ノズルから吐出させた後、表１に示す温度の乾燥空間（距離１０ｃｍ）を通して乾燥させ、表１に示す温度の水（外部凝固液）が入った凝固槽に通過させた。
その後、さらに４０℃の水が入った水洗槽を通過させて溶媒を洗浄除去し、中空糸型膜を巻き取った。
巻き取った中空糸膜を９０℃の恒温水槽に入れ、1時間熱収縮させた。その後、４０質量％のグリセリン水浴に３時間浸漬させた後、５５℃の乾燥機で４時間乾燥させた。
得られた中空糸膜について、上記した各測定を実施した。結果を表１に示す。
また実施例１と比較例１の中空糸膜の断面構造のＳＥＭ写真を図１、図２に示す。 <Manufacture of hollow fiber type semipermeable membrane>
The film forming solution composition was allowed to stand at 80 ° C. for 15 hours for degassing.
Using the defoamed membrane-forming solution composition, extrusion spinning was performed from a double spinning nozzle heated to 50 ° C. The internal coagulation liquid shown in Table 1 was used.
After discharging from the double spinning nozzle, it was dried through a drying space (distance 10 cm) at the temperature shown in Table 1 and passed through a coagulation tank containing water (external coagulation liquid) at the temperature shown in Table 1.
Thereafter, the solvent was washed and removed by passing through a washing tank containing 40 ° C. water, and the hollow fiber membrane was wound up.
The wound hollow fiber membrane was placed in a constant temperature water bath at 90 ° C. and heat-shrinked for 1 hour. Then, after being immersed in a 40% by mass glycerin water bath for 3 hours, it was dried with a dryer at 55 ° C. for 4 hours.
Each measurement mentioned above was implemented about the obtained hollow fiber membrane. The results are shown in Table 1.
Moreover, the SEM photograph of the cross-sectional structure of the hollow fiber membrane of Example 1 and Comparative Example 1 is shown in FIGS.

実施例１と比較例１の対比から、主にマクロボイドの面積割合の違いから、実施例１は透水性能とエンドトキシン阻止性能の両方が優れていたが、比較例１は透水性能が大きく劣っていた。   From a comparison between Example 1 and Comparative Example 1, mainly from the difference in the area ratio of macrovoids, Example 1 was excellent in both water permeability and endotoxin blocking performance, but Comparative Example 1 was greatly inferior in water permeability. It was.

本発明の中空糸膜は、純水透過係数が高く、エンドトキシン阻止性能も高いことから、医療用や工業用のエンドトキシン捕捉フィルターとして利用できる。   Since the hollow fiber membrane of the present invention has a high pure water permeability coefficient and a high endotoxin blocking performance, it can be used as an endotoxin capture filter for medical use or industrial use.

Claims (4)

中空糸膜成分中の８０質量％以上がポリエーテルスルホンであり、
中空糸膜断面に最大径が１０μｍ以上のマクロボイドを有し、前記マクロボイドの中空糸膜断面積に占める面積割合が２０〜４０％であり、
純水透過係数（ＰＷＰ）が１６００L／m2・h(0.1MPa)以上で、エンドトキシン濃度が１００ＥＵ/ｍｌの試験液を用い、JIS K3824に準じて測定されたエンドトキシン阻止性能（ＥＴ ＬＲＶ）が３以上である、エンドトキシン捕捉フィルター用中空糸膜。 80 mass% or more of the hollow fiber membrane component is polyethersulfone,
The cross section of the hollow fiber membrane has a macro void having a maximum diameter of 10 μm or more, and the area ratio of the macro void to the cross section of the hollow fiber membrane is 20 to 40%.
The endotoxin blocking performance (ET LRV) measured according to JIS K3824 using a test solution with a pure water permeability coefficient (PWP) of 1600 L / m 2 · h (0.1 MPa) or more and an endotoxin concentration of 100 EU / ml is 3 The above is a hollow fiber membrane for an endotoxin capture filter. 請求項１記載のエンドトキシン捕捉フィルター用中空糸膜の紡糸工程を含む製造方法であって、
前記紡糸工程において、内部凝固液として、水、ポリエチレングリコールおよびジメチルスルホキシドの混合溶液を使用する、エンドトキシン捕捉フィルター用中空糸膜の製造方法。 A production method comprising a spinning step of a hollow fiber membrane for an endotoxin capture filter according to claim 1,
A method for producing a hollow fiber membrane for an endotoxin-capturing filter, wherein, in the spinning step, a mixed solution of water, polyethylene glycol and dimethyl sulfoxide is used as an internal coagulation liquid. ポリエーテルスルホン、ジメチルスルホキシドおよびポリエチレングリコールを含む製膜溶液組成物を使用する、請求項２記載のエンドトキシン捕捉フィルター用中空糸膜の製造方法。   The method for producing a hollow fiber membrane for an endotoxin-capturing filter according to claim 2, wherein a membrane-forming solution composition containing polyethersulfone, dimethylsulfoxide and polyethylene glycol is used. 前記内部凝固液が、水１５〜２５質量％、ポリエチレングリコール１５〜２５質量％およびジメチルスルホキシド５０〜７０質量％からなるものである、請求項２または３記載のエンドトキシン捕捉フィルター用中空糸膜の製造方法。   The production of a hollow fiber membrane for an endotoxin-capturing filter according to claim 2 or 3, wherein the internal coagulation liquid comprises 15 to 25% by mass of water, 15 to 25% by mass of polyethylene glycol, and 50 to 70% by mass of dimethyl sulfoxide. Method.
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JP2003210573A (en) * 2002-01-22 2003-07-29 Nikkiso Co Ltd Hollow fiber type blood-purifier, and manufacturing method for hollow fiber membrane
JP2004121608A (en) * 2002-10-03 2004-04-22 Toyobo Co Ltd Hollow fiber membrane for dialysis liquid purification, and method for producing the same
WO2005021068A1 (en) * 2003-08-29 2005-03-10 Toyo Boseki Kabushiki Kaisha Highly water-permeable blood purifier of hollow-fiber membrane type
JP2005305264A (en) * 2004-04-20 2005-11-04 Daicel Chem Ind Ltd Separation membrane for co2 collection
JP2008173163A (en) * 2007-01-16 2008-07-31 Nikkiso Co Ltd Blood purifier and method for producing the same
WO2016072409A1 (en) * 2014-11-04 2016-05-12 旭化成メディカル株式会社 Hollow fiber filtration membrane

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