JP6400885B2 - 複合半透膜の製造方法 - Google Patents
複合半透膜の製造方法 Download PDFInfo
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- JP6400885B2 JP6400885B2 JP2013090126A JP2013090126A JP6400885B2 JP 6400885 B2 JP6400885 B2 JP 6400885B2 JP 2013090126 A JP2013090126 A JP 2013090126A JP 2013090126 A JP2013090126 A JP 2013090126A JP 6400885 B2 JP6400885 B2 JP 6400885B2
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- porous support
- foreign matter
- composite semipermeable
- semipermeable membrane
- skin layer
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/107—Organic support material
- B01D69/1071—Woven, non-woven or net mesh
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
- B01D69/1251—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction by interfacial polymerisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/56—Polyamides, e.g. polyester-amides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Description
(MgSO4阻止率の測定)
作製したサンプルを平膜評価用のセルにセットした。0.2重量%のMgSO4を含みかつNaOHを用いてpH6.5に調整した水溶液を25℃で膜の供給側と透過側に0.9MPaの差圧を与えて膜に接触させ、該水溶液を30分間透過させた。この操作によって得られた透過水の電導度を測定し、MgSO4阻止率(%)を算出した。MgSO4阻止率は、MgSO4濃度と水溶液電導度の相関(検量線)を事前に作成し、それらを用いて下式により算出した。
MgSO4阻止率(%)={1−(透過液中のMgSO4濃度[mg/L])/(供給液中のMgSO4濃度[mg/L])}×100
作製したサンプルを平膜評価用のセルにセットした。1重量%のベーシックバイオレット染料を含む水溶液を25℃で膜の供給側と透過側に1.5MPaの差圧を与えて膜に接触させ、該水溶液を10分間透過させ、染料を膜面に付着させた。
ロール状に巻かれた多孔性支持体(不織布上にポリスルホン多孔層を形成したUF膜)を連続的に送り出しながら、多孔性支持体の両面に10L/(min・m)の純水を1秒間吹き付け、その直後にフッ素ゴムブレードワイパー(タイプA硬度:50)を多孔性支持体のスキン層形成面に接触させて異物を除去した(異物除去工程)。ここで、多孔性支持体からサンプル(10mm×10mm)を幅方向に適正量切り取り、顕微鏡を用いて目視にて50nm以上の微粒子の数を数え、その平均値を求めた。その結果を表1に示す。
その後、残った多孔性支持体に対して、ピペラジン1.2重量%を含有するアミン水溶液をその表面に塗布し、その後余分なアミン水溶液を除去することにより水溶液被覆層を形成した。次に、前記水溶液被覆層の表面にトリメシン酸クロライド0.9重量%を含有するイソオクタン溶液を塗布した。その後、余分な溶液を除去し、さらに120℃の熱風乾燥機中で3分間保持して、多孔性支持体上にポリアミド系樹脂を含むスキン層を形成して複合半透膜を得た。このときの初期(製膜0〜1m)及び製膜位置1000mの複合半透膜からφ75mmの大きさのサンプルをそれぞれ3枚ずつ切り取り、該サンプルを用いてMgSO4阻止率の測定を行った。その結果の平均値を表1に示す。
実施例1の異物除去工程において、多孔性支持体の両面に10L/(min・m)の純水を1秒間吹き付けた後に、多孔性支持体の両面に風速40m/sの空気を1秒間吹き付けて異物を除去したこと以外は実施例1と同様の方法で複合半透膜を作製し、MgSO4阻止率の測定を行った。その結果の平均値を表1に示す。
実施例1の異物除去工程において、多孔性支持体の両面に風速40m/sの空気を1秒間吹き付けた後に、実施例1と同様にゴムブレードワイパーで処理して異物を除去したこと以外は実施例1と同様の方法で複合半透膜を作製し、MgSO4阻止率の測定を行った。その結果の平均値を表1に示す。
実施例1の異物除去工程において、多孔性支持体の両面に風速40m/sの空気を1秒間吹き付ける処理を連続的に2回施して異物を除去したこと以外は実施例1と同様の方法で複合半透膜を作製し、MgSO4阻止率の測定を行った。その結果の平均値を表1に示す。
実施例1の異物除去工程において、多孔性支持体の両面に10L/(min・m)の純水を1秒間吹き付けて異物を除去した後、多孔性支持体を傾斜させて余剰水分を除去したこと以外は実施例1と同様の方法で複合半透膜を作製し、MgSO4阻止率の測定を行った。その結果の平均値を表1に示す。
実施例1の異物除去工程において、多孔性支持体の両面に1L/(min・m)の純水を1秒間吹き付けて異物を除去した後、多孔性支持体を傾斜させて余剰水分を除去したこと以外は実施例1と同様の方法で複合半透膜を作製し、MgSO4阻止率の測定を行った。その結果の平均値を表1に示す。
実施例1の異物除去工程において、多孔性支持体の両面に0.5L/(min・m)の純水を1秒間吹き付けて異物を除去した後、多孔性支持体を傾斜させて余剰水分を除去したこと以外は実施例1と同様の方法で複合半透膜を作製し、MgSO4阻止率の測定を行った。その結果の平均値を表1に示す。
実施例1の異物除去工程を行わなかったこと以外は実施例1と同様の方法で複合半透膜を作製し、MgSO4阻止率の測定を行った。その結果の平均値を表1に示す。
Claims (6)
- スキン層を多孔性支持体の表面に形成してなる水処理用複合半透膜の製造方法において、スキン層を多孔性支持体の表面に形成する前に、多孔性支持体の表面に付着している最大幅が50nm以上の微粒子である異物を除去する異物除去工程を含み、
前記異物除去工程は、多孔性支持体表面への液体吹き付け処理、多孔性支持体表面でのワイパー、スキージ又はブラシの接触移動処理、多孔性支持体表面への気体吹き付け処理、又はこれらの2種以上の組み合わせにより行い、
前記スキン層は、多官能アミン成分と多官能酸ハライド成分とを重合してなるポリアミド系樹脂を含むものであり、多官能アミン成分を含むアミン水溶液を多孔性支持体の表面に接触させる前に、前記異物除去工程を行うことを特徴とする水処理用複合半透膜の製造方法。 - 前記異物除去工程は、液体吹き付け処理をした後、接触移動処理又は気体吹き付け処理を行う工程である請求項1記載の水処理用複合半透膜の製造方法。
- 前記異物除去工程は、気体吹き付け処理をした後、接触移動処理を行う工程である請求項1記載の水処理用複合半透膜の製造方法。
- 前記異物除去工程は、多孔性支持体の両側表面に付着している異物を除去する工程である請求項1〜3のいずれかに記載の水処理用複合半透膜の製造方法。
- 前記異物除去工程は、アミン水溶液を多孔性支持体の表面に接触させる前、60秒以内に行う請求項1〜4のいずれかに記載の水処理用複合半透膜の製造方法。
- 前記多官能アミン成分が、脂環式多官能アミンである請求項1〜5のいずれかに記載の水処理用複合半透膜の製造方法。
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