JP5946909B2 - 逆浸透分離膜の製造方法及びそれにより製造された逆浸透分離膜 - Google Patents
逆浸透分離膜の製造方法及びそれにより製造された逆浸透分離膜 Download PDFInfo
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- JP5946909B2 JP5946909B2 JP2014516934A JP2014516934A JP5946909B2 JP 5946909 B2 JP5946909 B2 JP 5946909B2 JP 2014516934 A JP2014516934 A JP 2014516934A JP 2014516934 A JP2014516934 A JP 2014516934A JP 5946909 B2 JP5946909 B2 JP 5946909B2
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- reverse osmosis
- separation membrane
- solvent
- dimethylformamide
- osmosis separation
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- 229920000515 polycarbonate Polymers 0.000 description 1
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- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920005649 polyetherethersulfone Polymers 0.000 description 1
- 229920001955 polyphenylene ether Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- LXEJRKJRKIFVNY-UHFFFAOYSA-N terephthaloyl chloride Chemical compound ClC(=O)C1=CC=C(C(Cl)=O)C=C1 LXEJRKJRKIFVNY-UHFFFAOYSA-N 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/025—Reverse osmosis; Hyperfiltration
-
- 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
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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
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/1216—Three or more layers
-
- 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
-
- 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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/12—Specific ratios of components used
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/219—Specific solvent system
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
- B01D2325/0283—Pore size
- B01D2325/02833—Pore size more than 10 and up to 100 nm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2350/00—Pretreatment of the substrate
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Description
DMF(N,N−Dimethylformamide、DMFの溶解度パラメーター:24.9(J/cm3)1/2)とDMSO(Dimethyl Sulfoxide、DMSOの溶解度パラメーター:26.7(J/cm3)1/2)を90:10比率で混ぜた混合溶媒に、18wt%ポリスルホンを入れて80℃で12時間以上攪拌し均一な液相を得た。上記溶液をポリエステル材質の100μm不織布上に総厚さが150μmになるようキャスティングした後、水に浸漬させて、多孔性ポリスルホン支持体を形成した。
DMF:DMSOを80:20の比率で混ぜた混合溶媒を使用したことを除き、実施例1と同様の過程で逆浸透分離膜を製作した。
DMF:DMSOを70:30の比率で混ぜた混合溶媒を使用したことを除き、実施例1と同様の過程で逆浸透分離膜を製作した。
DMF:DMSOを60:40の比率で混ぜた混合溶媒を使用したことを除き、実施例1と同様の過程で逆浸透分離膜を製作した。
DMF:DMSOの混合溶媒の代わりにDMF:GBL(γ−butyrolactone、GBLの溶解度パラメーター:25.6(J/cm3)1/2)を90:10の比率で混ぜた混合溶媒を使用し、また、上記混合溶媒に16wt%ポリスルホンを入れたことを除き、実施例1と同様の過程で逆浸透分離膜を製作した。
DMF:DMSOの混合溶媒の代わりにDMF:GBLを80:20の比率で混ぜた混合溶媒を使用し、また、上記混合溶媒に16wt%ポリスルホンを入れたことを除き、実施例1と同様の過程で逆浸透分離膜を製作した。
DMF:DMSOの混合溶媒の代わりにDMF:GBLを70:30の比率で混ぜた混合溶媒を使用し、また、上記混合溶媒に16wt%ポリスルホンを入れたことを除き、実施例1と同様の過程で逆浸透分離膜を製作した。
DMF:DMSOの混合溶媒の代わりにDMF:GBLを60:40の比率で混ぜた混合溶媒を使用し、また、上記混合溶媒に16wt%ポリスルホンを入れたことを除き、実施例1と同様の過程で逆浸透分離膜を製作した。
多孔性ポリスルホン支持体を形成する際にDMFのみを溶媒として使用したことを除き、実施例1と同様の過程で逆浸透分離膜を製作した。
多孔性ポリスルホン支持体を形成する際にDMFのみを溶媒として使用したことを除き、実施例5と同様の過程で逆浸透分離膜を製作した。
上記実施例1〜8及び比較例1〜2により製造された逆浸透分離膜の初期塩除去率及び初期透過流量を測定した。初期塩除去率と初期透過流量は、25℃で32,000ppmの塩化ナトリウム水溶液を、800psiで4500mL/minの流量で供給しながら測定した。膜評価に使用した逆浸透膜セル装置は、GE Osmosis社のSepa CF IIセルで、平板型透過セルと高圧ポンプ、貯蔵槽及び冷却装置を備えており、平板型透過セルの構造はクロスフロー(cross−flow)方式で、有効透過面積が140cm2である。洗浄した逆浸透分離膜を透過セルに設けた後、評価装置の安定化のために、3次蒸留水を利用して1時間程度十分な予備運転を行った。それから、32,000ppmの塩化ナトリウム水溶液に替えて圧力と透過流量が正常状態に至るまで1時間程度装置運転を行った後、8分〜10分間透過される水の量を測定して流量を計算し、伝導度メートル(Conductivity Meter)を用いて透過前後の塩濃度を分析し塩除去率を計算した。測定結果は、下[表1]及び[表2]に示した。
上記実施例1〜8及び比較例1〜2により製造された逆浸透分離膜の耐汚染性を評価した。耐汚染性評価は、32,000ppmのNaCl水溶液と100ppmのカゼイン混合水溶液を使用し、800psiの圧力で測定した。初期塩除去率及び流量を評価した後、100ppmのカゼイン水溶液を評価器のタンクに投入し、直ちに塩除去率と流量の変化を測定した。それから2時間後に塩除去率と流量の変化を測定した。カゼインはpH11以上の水溶液に溶かして使用した。測定結果は、[表3]に示した。
実施例1〜8及び比較例1〜2により製造された逆浸透分離膜において、ポリスルホン層の表面に形成された気孔のサイズ別の分布度を測定した。このとき、気孔のサイズ別の分布度は、ポリスルホン層の表面の面積1.27μm×0.83μmに対して測定した。また、測定は、image−Pro Plusを用いてSEM写真のコントラスト値を80に補正した後、補正したイメージをcount/size機能を利用して行った。その結果は、下表4に示した通りである。
Claims (5)
- 多孔性支持体の一面に異なる溶解度パラメーター値を有する第1溶媒及び第2溶媒を含有する混合溶媒を含む溶液を接触させてポリスルホン層を形成する段階と、
前記ポリスルホン層が形成された多孔性支持体上に活性層を形成する段階と、を含み、
前記第1溶媒は、DMFであり、かつ、
前記第2溶媒は、ジメチルアセトアミド(Dimethyl acetamide)、メチルアセテート(Methyl acetate)、ヒドラジン(Hydrazine)、卜リクロロメタン(Trichloromethane)、ジヨードメタン(Diiodomethane)、トリクロロエチレン(Trichloroethylene)、スチレン(Styrene)、2−ブタノン(2−Butanone)、テトラヒドロフラン(Tetrahydrofuran)、シクロヘキサノン(Cyclohexanone)、アセトン(Acetone)、ベンゾニトリル(Benzonitrile)、イソホロン(Isophorone)、2−エチル−1−ヘキサノール(2−Ethyl−1−hexanol)、ジクロロメタン(Dichloromethane)、ジブチルフタレート(Dibutyl phthalate)、1,4−ジオキサン(1,4−Dioxane)、1,2−ジクロロベンゼン(1,2−Dichlorobenzene)、1,2−ジクロロエタン(1,2−Dichloroethane)、2−ブトキシエタノール(2−Butoxyethanol)、1−ブロモナフタレン(1−Bromonaphthalene)、アセト酸(Acetic acid)、エピクロロヒドリン(Epichlorohydrin)、ベンズアルデヒド(Benzaldehyde)、モルホリン(Morpholine)、アクリロニトリル(Acrylonitrile)、アセトフェノン(Acetophenone)、ピリジン(Pyridine)、2−ブタノール(2−Butanol)、シクロヘキサノール(Cyclohexanol)、アニリン(Aniline)、2−メチルプロピルアルコール(2−Methylpropyl alcohol)、3−メチルフェノール(3−Methylphenol)、N−メチル−2−ピロリジン(N−Methyl−2−pyrrolidine)、1−ブタノール(1−Butanol)、ブロミン(Bromine)、2−エトキシエタノール(2−Ethoxyethanol)、フェノキシエタノール(Phenoxyethanol)、2−プロパノール(2−Propanol)、ベンジルアルコール(Benzyl alcohol)、ジメチルエタノールアミン(Dimethylethanolamine)、2−フランメタノール(2−Furanmethanol)、アセトニトリル(Acetonitrile)、1−プロパノール(1−Propanol)、2−メトキシメタノール(2−Methoxymethanol)、メタン酸(Methanoic acid)、N,N−ジメチルホルムアミド(N,N−Dimethylformamide)、ニトロメタン(Nitromethane)、エタノール(Ethanol)、ジメチルスルホキシド(Dimethyl sulfoxide)、プロピレンカーボネート(Propylene carbonate)、1,3−ブタンジオール(1,3−Butanediol)、ジエチレングリコール(Diethylene glycol)、メタノール(Methanol)、1,2−プロパンジオール(1,2−Propanediol)、2−アミノエタノール(2−Aminoethanol)、エチレングリコール(Ethylene glycol)、エチレンカーボネート(Ethylene carbonate)、ジエチルスルフェート(Diethyl sulfate)、ニトロエタン(Nitroethane)、アリルアルコール(Allyl alcohol)及びγ−ブチロラクトン(γ−butyrolactone)からなる群より選択され、
前記第1溶媒及び前記第2溶媒との溶解度パラメーター値の差が0.1(J/cm 3 ) 1/2 〜3(J/cm 3 ) 1/2 であり、
前記混合溶媒は、90:10〜60:40の比率の前記第1溶媒及び前記第2溶媒を含むことを特徴とする逆浸透分離膜の製造方法。 - 前記混合溶媒は、N、N−ジメチルホルムアミド(N、N−Dimethylformamide、DMF)及びジメチルスルホキシド(Dimethyl sulfoxide、DMSO)の混合溶媒である、請求項1に記載の逆浸透分離膜の製造方法。
- 前記混合溶媒は、N、N−ジメチルホルムアミド(N、N−Dimethylformamide、DMF)及びγ−ブチロラクトン(γ−butyrolactone、GBL)の混合溶媒である、請求項1に記載の逆浸透分離膜の製造方法。
- 前記混合溶媒は、N、N−ジメチルホルムアミド(N、N−Dimethylformamide、DMF)及びジメチルスルホキシド(Dimethyl sulfoxide、DMSO)を90:10〜60:40の比率で混合したものである、請求項1に記載の逆浸透分離膜の製造方法。
- 前記混合溶媒は、N、N−ジメチルホルムアミド(N、N−Dimethylformamide、DMF)及びγ−ブチロラクトン(γ−butyrolactone、GBL)を95:5〜50:50の比率で混合したものである、請求項1に記載の逆浸透分離膜の製造方法。
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EP2857088A1 (en) | 2015-04-08 |
US20150114902A1 (en) | 2015-04-30 |
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US20140014576A1 (en) | 2014-01-16 |
JP2014519411A (ja) | 2014-08-14 |
EP2857088B1 (en) | 2020-02-26 |
EP2857088A4 (en) | 2016-02-17 |
US8993053B2 (en) | 2015-03-31 |
US9643209B2 (en) | 2017-05-09 |
WO2013176523A1 (ko) | 2013-11-28 |
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