JP5837394B2 - シート状分離膜の製造方法 - Google Patents
シート状分離膜の製造方法 Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims description 103
- 238000000926 separation method Methods 0.000 title claims description 92
- 238000004519 manufacturing process Methods 0.000 title claims description 29
- 239000007788 liquid Substances 0.000 claims description 123
- 238000000034 method Methods 0.000 claims description 73
- 238000005345 coagulation Methods 0.000 claims description 63
- 230000015271 coagulation Effects 0.000 claims description 63
- 230000001112 coagulating effect Effects 0.000 claims description 50
- 239000002904 solvent Substances 0.000 claims description 40
- 239000000758 substrate Substances 0.000 claims description 40
- 238000000576 coating method Methods 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 16
- 229920000642 polymer Polymers 0.000 claims description 16
- 229920002492 poly(sulfone) Polymers 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 11
- 239000002033 PVDF binder Substances 0.000 claims description 7
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 7
- 239000000243 solution Substances 0.000 description 71
- 239000000463 material Substances 0.000 description 27
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 13
- 230000015572 biosynthetic process Effects 0.000 description 13
- 238000011156 evaluation Methods 0.000 description 13
- 239000010410 layer Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- 238000005191 phase separation Methods 0.000 description 9
- 239000002202 Polyethylene glycol Substances 0.000 description 8
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- 238000005259 measurement Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000004745 nonwoven fabric Substances 0.000 description 5
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 3
- 239000004734 Polyphenylene sulfide Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000001471 micro-filtration Methods 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920000069 polyphenylene sulfide Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000001223 reverse osmosis Methods 0.000 description 3
- 238000000108 ultra-filtration Methods 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 229920002301 cellulose acetate Polymers 0.000 description 2
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- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000012510 hollow fiber Substances 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002759 woven fabric Substances 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000005456 alcohol based solvent Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000004320 controlled atmosphere Methods 0.000 description 1
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- 239000010840 domestic wastewater Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229920001600 hydrophobic polymer Polymers 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005305 interferometry Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000009291 secondary effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
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Classifications
-
- 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
- B01D69/06—Flat membranes
-
- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
-
- 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
- B01D67/0095—Drying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
- B01D65/102—Detection of leaks in membranes
-
- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0016—Coagulation
- B01D67/00165—Composition of the coagulation baths
-
- 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
- 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
- B01D69/1213—Laminated layers
-
- 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
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/42—Details of membrane preparation apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/50—Control of the membrane preparation process
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Description
JIS K3832(ASTM F316−86)に準拠してバプルポイント圧力を測定する。製膜初期の分離膜について、幅方向に略均等な5点から直径25mmの円形サンプルを打ち抜き、次いで、前記サンプルの1つずつ、分離膜面側から窒素ガスを徐々に加圧しながら裏面側に満たした水面に連続的に気泡が生じる圧力(バブルポイント圧力)を確認する。このときの試験装置例を図6に示す。このとき、最大印加圧力は1MPaとし、1MPaにおいて気泡が発生しない場合のバブルポイント圧力は、「>1[MPa]」とした。
PBP(バブルポイント圧力 [MPa])=4・δ/d
(δ:水の表面張力≒72×10-3 [N/m]、d:最大孔径[μm])
このとき例えば、バブルポイント圧力が1MPaの時、最大孔径は約0.3μmとなる。
製膜後の膜面の外観を目視で観察して、凝固液のハジキに起因する外観の不均一状態、不均一な相分離に起因する外観の不均一状態などを、評価した。
得られたシート状分離膜より、幅方向において略均等な位置の3点(右側、中央、左側)から直径75mmで採取したサンプルを循環流通式平膜テストセルにより、下記の条件によって性能評価した。
測定条件としては、ポリエチレングリコール(和光純薬社製試薬1級、平均分子量20、000 Da)、原液濃度:0.5%、原液温度:25℃を評価物質として、圧力:0.35MPa、循環流量:10 L/min.により測定した。
この測定について、製膜開始直後を製膜時間0分とし、以後、30、60、90、120、240、360、500、750、1000分製膜した時の分離膜サンプルについて同様の測定を行い、それぞれ製膜時間0分との変化率(各製膜時間の阻止率/製膜時間0分の阻止率×100[%])を求めた結果をグラフに表した。実施例1、2および比較例1の結果を図1に示す。
ポリスルホン(ソルベイ アドバンスト ポリマーズ社製、Udel P−3500)18.3重量%をジメチルホルムアミド81.7重量%と混合し、100℃で溶解・濾過・脱泡して製膜溶液を調製した。この製膜溶液を、約25℃に保ちつつ、ライン速度60m/minで、多孔性基材であるポリエステル製不織布(坪量70g/m2、厚み90um、幅280mm)に、塗布幅250mmのスロットダイコータでWet塗布厚み130μmとなるように塗布した。
実施例1において、凝固液として30℃の40%DMF水溶液を塗布した以外は実施例1と同様にして厚み130μmのシート状分離膜を得た。このシート状分離膜について、前記評価を行った結果を表1、及び図1に示す。
実施例1において、凝固液塗布後の傾斜下降角度を80°にし、保持時間が0.3secであった以外は実施例1と同様にして厚み130μmのシート状分離膜を得た。このシート状分離膜について、前記評価を行った結果を表1に示す。
実施例1において、ライン速度を30m/minとし、凝固液塗布厚みが1mmであった以外は実施例1と同様にして厚み130μmのシート状分離膜を得た。このシート状分離膜について、前記評価を行った結果を表1に示す。
実施例1において、凝固液塗布直後の傾斜下降角度を90°にした以外は実施例1と同様にして厚み130μmのシート状分離膜を得た。このシート状分離膜について評価した結果を表1に示す。
実施例1において、凝固の方法として液膜落下方式で塗布する代わりに、20℃の純水を満たした槽に浸漬させる以外は実施例1と同様にして厚み130μmのシート状分離膜を得た。このシート状分離膜について、前記評価を行った結果を表1、及び図1に示す。
実施例1において、凝固液塗布方法として、下部からスロットダイコータにて凝固液をWet厚み約0.5mmになるように塗布した以外は実施例1と同様にして厚み130μmのシート状分離膜を得た。このシート状分離膜について、前記評価を行った結果を表1、及び図2に示す。
実施例1において、製膜溶液塗布後に90°で下降するように傾斜させるとともに、横向きのスロットダイコータを用いて実施例1と同様の凝固液を接触塗布した以外は実施例1と同様にして厚み130μmのシート状分離膜を得た。このシート状分離膜について評価した結果を表1に示す。
4 製膜溶液タンク
6 ダイコータ
7 調湿空間
9 凝固液タンク
11 ダイコータ
15 洗浄槽
A 調湿雰囲気ガス
B 基材
D1 搬送方向(調湿工程)
D2 搬送方向(凝固液塗布工程)
Claims (6)
- 多孔性基材上に微多孔性層を形成したシート状分離膜の製造方法において、ポリマーを溶媒に溶解した製膜溶液を多孔性基材上に塗布する製膜溶液塗布工程と、製膜溶液が塗布された多孔性基材に液膜落下方式により凝固液を塗布する凝固液塗布工程と、凝固した微多孔性層から溶媒を除去する溶媒除去工程とを有し、前記凝固液塗布工程は、下流側を低くした傾斜部に前記多孔性基材を搬送しながら、傾斜部において、前記多孔性基材上に凝固液を落下させる工程であり、前記傾斜部は、水平方向に対する傾斜角度が30〜80°であることを特徴とするシート状分離膜の製造方法。
- 前記傾斜部において、前記多孔性基材は支持ロールで下方から支持されている請求項1に記載のシート状分離膜の製造方法。
- 前記製膜溶液塗布工程と凝固液塗布工程の間に、前記製膜溶液を調湿雰囲気と接触させる調湿工程をさらに有する請求項1又は2に記載のシート状分離膜の製造方法。
- 前記調湿工程は、製膜溶液が塗布された前記多孔性基材を調湿空間中で搬送しながら、その搬送方向に沿って逆方向に調湿雰囲気ガスを流動させるカウンターフロー方式で行われる請求項3記載のシート状分離膜の製造方法。
- 前記製膜溶液が、ポリスルホンまたはポリフッ化ビニリデンを含む請求項1〜4のいずれかに記載のシート状分離膜の製造方法。
- 前記凝固液塗布工程における凝固液の塗布速度が、20m/min以上である請求項1〜5のいずれかに記載のシート状分離膜の製造方法。
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US10421111B2 (en) | 2015-04-17 | 2019-09-24 | Ball Corporation | Method and apparatus for controlling an operation performed on a continuous sheet of material |
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JP6577781B2 (ja) * | 2015-08-03 | 2019-09-18 | 株式会社クラレ | 中空糸膜、及び中空糸膜の製造方法 |
CN105344246A (zh) * | 2015-10-23 | 2016-02-24 | 蓝星(成都)新材料有限公司 | 一种超滤膜及其制备方法 |
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