JP7046867B2 - 液体をろ過するための中空繊維膜 - Google Patents
液体をろ過するための中空繊維膜 Download PDFInfo
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- JP7046867B2 JP7046867B2 JP2019087760A JP2019087760A JP7046867B2 JP 7046867 B2 JP7046867 B2 JP 7046867B2 JP 2019087760 A JP2019087760 A JP 2019087760A JP 2019087760 A JP2019087760 A JP 2019087760A JP 7046867 B2 JP7046867 B2 JP 7046867B2
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- polymer
- antibacterial
- hollow fiber
- membrane
- essentially
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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Description
a)ポリマーまたはポリマー混合物をPEG(分子量‐300)を含む細孔形成剤と混合するステップと、
b)ステップa)において製造した混合物をポリマー用の非溶媒と共に紡糸口金に通過させるステップと、
を含む、固有の抗菌性中空繊維膜を製造する方法が提供される。
a)抗菌物質埋め込みポリマーまたは抗菌物質埋め込みポリマー混合物、抗菌物質を含まないポリマーまたはポリマー混合物、ポリマーまたはポリマー混合物両方のための溶媒、およびPEG(分子量‐300)を含む細孔形成剤を混合するステップと、
b)ステップa)において製造した混合物をポリマー用の非溶媒と共に紡糸口金に通過させるステップと、
を含み得る。
a)抗菌物質埋め込みポリマーまたは抗菌物質埋め込みポリマー混合物を、抗菌物質を含まないポリマーまたはポリマー混合物および両方のポリマー用の溶媒と、PEG、LiCl、PVPなどのその他の添加物とともに混合するステップと、
b)ステップa)において製造した混合物をポリマー用の非溶媒と共に紡糸口金に通過させるステップと、
を含む固有の抗菌性中空繊維膜を製造する方法が提供される。
本発明の好ましい実施形態を例示目的で説明してきたが、本発明の精神または範囲から逸脱することなく本発明において様々な修正、追加、および置換を行うことができることは当業者には明らかであろう。したがって、本発明は、添付の特許請求の範囲およびそれらの均等物の範囲内にある限り、本発明の修正形態および変形形態を網羅することが意図されている。
以下の表中の成分を組み合わせることによってドープ溶液/ポリマー溶液を調製した。これに、下記のボア溶液/内部溶液を添加し、そしてその組み合わせを完全に混合した。次いで、この混合物を水と共に紡糸口金に通過させて中空繊維を形成した。
1.ドープ溶液を製造するプロセスにおいて、低分子量添加剤(例えばLiClなど)を最初に溶媒中に絶えず撹拌しながら50℃で添加する。
2.徐々に、分子量の大きい添加剤(PEG、PVPなど)を一定に撹拌しながら溶媒に添加する。
3.最後に、ベースポリマー(例えばPES、PSUなど)をドープ溶液中に一定に撹拌しながら80℃で約3時間導入する。
4.ドープ溶液は、すべての添加剤とベースポリマーが溶媒に均一に溶解することで紡糸の準備が整ったとみなされる。ドープ溶液は、紡糸前に気泡および異物が存在しない状態で、一相である。
5.攪拌中に発生する気泡を除去するために、ドープ溶液を一晩または十分な時間撹拌せずに放置する。
6.紡糸口金の温度は室温であるが、凝固液の温度は50℃である。
7.ボア溶液は、純粋なPEG、またはPEG:水9:1またはNMP:水9:1の混合物のいずれかであり得る。
純水流束実験は脱イオン水を用いて行った。各モジュールを脱イオン水に24時間浸し、試験システム内で1 1/2時間運転して、サンプル採取前に中空糸膜に対する残留グリセロールの影響を排除した。PWPおよびタンパク質除去を評価するために設計されたUF実験装置が詳細に示されている(CS Feng、B. Shi、G. Li、Y. Wu、Preparation and properties of microporous membrane from polyvinylidene fluoride cotetrafluoroethylene) (F2.4) for membrane distillation、J. Membr. Sci. 237 (2004) 15‐24参照)。1barの膜貫通圧力および20℃の供給溶液温度で、全ての実験は直交流モードで中空繊維モジュールにおいて行った。各中空繊維サンプルにつき2つのモジュールを調製した。
純水透過流束(PWP)は以下のようにして得た。
Table 1:
Tableは、調製された10個の中空繊維膜サンプルについて行われたPWP試験の間に記録されたデータを列挙する。
Flux Tables-10サンプルからの5対
Table 2は、各膜について120分の時間にわたって5分間隔で確立された純水流束の概要を提供する。結果は図8にも示す。
実施例2に従って製造された中空繊維を有する膜を提供したが、ポリマー内に亜鉛塩を埋め込んだ。我々のケースではポリエーテルスルホンである、繊維を作製するための主要なポリマーは、亜鉛ピリチオンなどの亜鉛の塩を使用して修飾される。この修飾は、US9527918に記載されている方法に基づいて行われる。
次いで、膜を、ポリマー表面の抗菌性を評価するための標準的な国際的方法を用いて、2種類の細菌株(大腸菌ATCC 8739(グラム-)および黄色ブドウ球菌6538(グラム+))を阻害する能力について試験した。結果は、ペトリ皿上で増殖した細菌培養物の画像に見出すことができ、図9に示す。結果を以下に提供する。
上記のように調製された抗菌性ポリマーポリエーテルスルホンを紡糸することによって得られた中空繊維を試験して、皮膚と接触することを意図したプラスチック製品に関する現在の法令によって定義された主要微生物株に対するポリマーの有効性を評価した。
非多孔性プラスチック表面の抗菌活性を評価するための標準的な国際的方法を用いて、2種類の細菌株(大腸菌ATCC8739(グラム-)および黄色ブドウ球菌ATCC6538(グラム+))について製品を試験した。
成形初期インキュベーション対照ポリマー37℃でのMICROBIAL接種材料接種項目還元株(cfu/ml)24時間(cfu/ml)(cfu/ml)log還元%エシェリキア2.5×106 6.2×107 1.0×107 0.79 83.87%黄色ブドウ球菌1.7×106 2.3×107 1.4×106 1.2 93.91%アウレウス
得られた結果は、37℃で24時間インキュベートした後に、亜鉛で処理したポリマーが細菌数を83.870(大腸菌の場合)および93.91%(黄色ブドウ球菌の場合)減少させることを示している。
図からわかるように、各3個の2セットで合計6個のペトリ皿がある。
上の3つはその物質に殺菌物性を与えるために銀ナノ粒子を含浸させた物質を有し、下の3つは本発明の繊維表面から抽出されたサンプル(紡糸中空繊維膜)を有する。上の3つのペトリ皿ではナノ粒子が浸出し、物質の外に移動/浸出してサンプル周囲の細菌を殺菌したことが分かる。しかしながら、下の3つのペトリ皿中の細菌増殖はサンプルの表面でのみ阻害され、抗菌性を付与する原因となる物質が本発明の材料から浸出しないという主張を裏付けるものである。
2 中空繊維
3 繊維端部
4 注封モジュール
5 ろ過された液体
6 繊維壁の空洞
7 親水性層
8 両方の層の合流点
9 液体と繊維との間の空間
10 粗粒子、汚染物
11 疎水性層
12 ろ過されていない液体
13 中空繊維の端部
14 注封モジュール壁
15 封止剤
Claims (31)
- 複数の多孔質中空膜繊維を含む液体ろ過用の固有の抗菌性中空繊維膜であって、前記中空膜繊維が、本質的に抗菌性を有し、抗菌物質が埋め込まれたポリマーから形成されており、前記中空繊維膜が、液体が繊維膜の外側から入り、多孔質膜を通って繊維の内腔に入りそこに沿って通過し、それにより保持液が膜の外側に残り、ろ過された液体(ろ液)が前記繊維の中空端から流出するように構成された、本質的に抗菌性の中空繊維膜。
- 前記中空繊維がポリマー、任意選択的に熱可塑性ポリマーから形成される、請求項1に記載の本質的に抗菌性の中空繊維膜。
- 前記繊維が、12%から25%のポリエーテルスルホン、5から20%のポリビニルピロリドン、70%から90%のN‐メチルピロリドン溶液、および10%から45%のポリエチレングリコールを含むかまたはそれらからなり、任意選択的に、前記繊維は、ポリカーボネート、ポリアミド、および水性イソプロピル、またはそれらの任意の組み合わせをさらに含む、請求項1または2に記載の本質的に抗菌性の中空繊維膜。
- 前記繊維が、10%から25%のポリスルホンおよび5%から15%のポリビニルピロリドンを含むかまたはそれらからなる、請求項1または2に記載の本質的に抗菌性の中空繊維膜。
- 前記繊維が、3%から25%のポリエーテルスルホンおよび5%から15%のポリビニルピロリドンを含むかまたはそれらからなる、請求項1または2に記載の本質的に抗菌性の中空繊維膜。
- 前記繊維が本質的に抗菌性である、請求項1から5のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 前記繊維が単層膜を形成し、前記単層膜が疎水性または親水性のいずれかである、請求項1に記載の本質的に抗菌性の中空繊維膜。
- 前記繊維が二層膜を形成し、前記二層膜が疎水性または親水性のいずれかである、請求項1に記載の本質的に抗菌性の中空繊維膜。
- 疎水性の層が空気捕捉および吸引圧力の要件を低減する、請求項1から8のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 疎水性の層が液体の流束を増加させる、請求項1から9のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 親水性の層が、繊維壁上の細孔を通って繊維の中空空洞に向かう液体の毛管作用を維持し、吸引圧力または通過圧力または重力ヘッドの要件を低減する、請求項1から10のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 液体が外側から内側への向きに流れる、請求項1から11のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 保持液が膜の外側に保持される、請求項1から12のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 膜が洗浄可能である、請求項1から13のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 前記中空繊維膜が、繊維壁の80体積%から90体積%の多孔率範囲を有する繊維を含む、請求項1から14のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 前記中空繊維膜の細孔が直径1nmから25nmの範囲を有する、請求項1から15のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 前記中空繊維が開口端を有するU字型の膜モジュールを形成し、ろ過のために液体が膜に入り、ろ過された液体が繊維の前記開口端を通って出る、請求項1から16のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 前記抗菌物質が、金属酸化物、金属塩または金属、例えば亜鉛塩である、請求項1に記載の本質的に抗菌性の中空繊維膜。
- 前記抗菌物質がポリマーまたはポリマー混合物に埋め込まれている、請求項1から18のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 前記抗菌物質が埋め込まれたポリマーまたはポリマー混合物が、前記繊維の2から5重量%である、請求項18または19に記載の本質的に抗菌性の中空繊維膜。
- 抗菌物質を含まないポリマーまたはポリマー混合物が、前記繊維の95から98重量%である、請求項18から20のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- 抗菌性物質を含む、または含まないポリマーまたはポリマー混合物が、同じポリマーまたはポリマー混合物である、請求項18から21のいずれか一項に記載の本質的に抗菌性の中空繊維膜。
- a)ポリマーまたはポリマー混合物をPEGを含む細孔形成剤と混合するステップと、
b)ステップa)において製造した混合物をポリマー用の非溶媒と共に紡糸口金に通過させるステップと、
を含む、請求項1から22のいずれか一項に記載の本質的に抗菌性の中空繊維膜を製造する方法。 - a)抗菌物質が埋め込まれたポリマーまたは抗菌物質が埋め込まれたポリマー混合物を、抗菌物質を含まないポリマーまたはポリマー混合物および両方のポリマー用の溶媒と混合するステップと、
b)ステップa)において製造した混合物をポリマー用の非溶媒と共に紡糸口金に通過させるステップと、
を含む、請求項1から22のいずれか一項に記載の本質的に抗菌性の中空繊維膜を製造する方法。 - ステップb)を25から80°の温度で実施する、請求項23または24に記載の方法。
- 抗菌物質が埋め込まれたポリマーまたはポリマー混合物が、ステップa)において形成された混合物中のポリマーの総重量の2から5重量%である、請求項23から25のいずれか一項に記載の方法。
- 抗菌物質を含まないポリマーまたはポリマー混合物は、繊維の95から98重量%である、請求項23から26のいずれか一項に記載の方法。
- 抗菌物質が埋め込まれたポリマーがポリエーテルスルホンであり、抗菌物質を含まないポリマーまたはポリマー混合物がポリエーテルスルホンであり、ポリマーが3%対97%の重量比で提供される、請求項23から27のいずれか一項に記載の方法。
- 抗菌物質を含む、または含まないポリマーまたはポリマー混合物が、同じポリマーまたはポリマー混合物である、請求項23から28のいずれか一項に記載の方法。
- 抗菌物質は、ポリマー鎖間の架橋を介してその中に埋め込まれた金属酸化物粒子を有する、請求項23から29のいずれか一項に記載の方法。
- 前記膜が、少なくとも1つの供給チャネルと少なくとも1つの排出チャネルとを有するハウジング内に配置される、請求項1から22のいずれか一項に記載の中空繊維膜を備える液体ろ過のための装置。
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