JP6703522B2 - 膜の製造方法 - Google Patents
膜の製造方法 Download PDFInfo
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- JP6703522B2 JP6703522B2 JP2017507832A JP2017507832A JP6703522B2 JP 6703522 B2 JP6703522 B2 JP 6703522B2 JP 2017507832 A JP2017507832 A JP 2017507832A JP 2017507832 A JP2017507832 A JP 2017507832A JP 6703522 B2 JP6703522 B2 JP 6703522B2
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- membrane
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- membranes
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- B01D67/0016—Coagulation
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- 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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/80—Block polymers
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
- A23L2/72—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration
- A23L2/74—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration using membranes, e.g. osmosis, ultrafiltration
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- 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
- B01D67/0011—Casting solutions therefor
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- 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
- B01D71/52—Polyethers
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- 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
- B01D71/52—Polyethers
- B01D71/521—Aliphatic polyethers
- B01D71/5211—Polyethylene glycol or polyethyleneoxide
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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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- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
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- C08G75/23—Polyethersulfones
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/005—Processes for mixing polymers
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/00—Details relating to properties of membranes
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- B01D2325/0283—Pore size
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- C08G2340/00—Filter material
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/06—Polysulfones; Polyethersulfones
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2481/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2481/06—Polysulfones; Polyethersulfones
Description
a)コポリマーCを製造するステップであって、該コポリマーCが、少なくとも1種のポリアリーレンエーテルAのブロックとポリアルキレンオキシドPAOのブロックとを含み、該コポリマーC中のポリアルキレンオキシドPAOの含有量が、30質量%〜90質量%であり、かつコポリマーCは、溶剤L中で製造されて、溶液Sが得られるステップ、
b)少なくとも1種のポリマーPを含むドープ溶液Dを準備するステップ、
c)溶液Sとドープ溶液Dとを混合するステップ、
d)その溶液Sとドープ溶液Dとの混合物を、少なくとも1種の凝固剤と接触させることによって膜を製造するステップ
を含む、製造方法に関する。
t、qは、それぞれ独立して、0、1、2または3であり、
Q、T、Yは、それぞれ独立して、化学結合または−O−、−S−、−SO2−、S=O、C=O、−N=N−、−CRaRb−から選択される基であり、ここでRaおよびRbは、それぞれ独立して、水素原子またはC1〜C12−アルキル、C1〜C12−アルコキシもしくはC6〜C18−アリール基であり、その際、Q、TおよびYの少なくとも1つは、−O−ではなく、かつQ、TおよびYの少なくとも1つは、−SO2−であり、かつ
Ar、Ar1は、それぞれ独立して、6〜18個の炭素原子を有するアリーレン基であり、
Dは、化学結合または−O−である]のポリアリーレンエーテル単位から形成することができる。
− Yは、ハロゲン原子であり、
− Xは、ハロゲン原子およびOHから、好ましくはハロゲン原子、特にF、ClまたはBrから選択され、かつ
− ArおよびAr1は、それぞれ独立して、6〜18個の炭素原子を有するアリーレン基である。
− ジヒドロキシベンゼン、特にヒドロキノンおよびレゾルシノール、
− ジヒドロキシナフタレン、特に1,5−ジヒドロキシナフタレン、1,6−ジヒドロキシナフタレン、1,7−ジヒドロキシナフタレンおよび2,7−ジヒドロキシナフタレン、
− ジヒドロキシビフェニル、特に4,4’−ビフェノールおよび2,2’−ビフェノール、
− ビスフェニルエーテル、特にビス(4−ヒドロキシフェニル)エーテルおよびビス(2−ヒドロキシフェニル)エーテル、
− ビスフェニルプロパン、特に2,2−ビス(4−ヒドロキシフェニル)プロパン、2,2−ビス(3−メチル−4−ヒドロキシフェニル)プロパンおよび2,2−ビス(3,5−ジメチル−4−ヒドロキシフェニル)プロパン、
− ビスフェニルメタン、特にビス(4−ヒドロキシフェニル)メタン、
− ビスフェニルスルホン、特にビス(4−ヒドロキシフェニル)スルホン、
− ビスフェニルスルフィド、特にビス(4−ヒドロキシフェニル)スルフィド、
− ビスフェニルケトン、特にビス(4−ヒドロキシフェニル)ケトン、
− ビスフェニルヘキサフルオロプロパン、特に2,2−ビス(3,5−ジメチル−4−ヒドロキシフェニル)ヘキサフルオロプロパン、ならびに、
− ビスフェニルフルオレン、特に9,9−ビス(4−ヒドロキシフェニル)フルオレン、
− 1,1−ビス(4−ヒドロキシフェニル)−3,3,5−トリメチルシクロヘキサン(ビスフェノールTMC)
から選択される。
略語:
DCDPS 4,4’−ジクロロジフェニルスルホン
DHDPS 4,4’−ジヒドロキシジフェニルスルホン
NMP N−メチルピロリドン
DMAc ジメチルアセトアミド
PWP 純水透過
MWCO 分子量カットオフ
粘度数(ISO 307、1157、1628;0.01g/モルのフェノール/1,2−オルトジクロロベンゼンの1:1溶液中)82、ガラス転移温度(DSC、10℃/分;ISO 11357−1/−2による)225℃、分子量Mw(DMAc中でのGPC、PMMA標準)75000g/モルを有するポリエーテルスルホン。
Luvitec(登録商標)K40
フィッケンチャーの方法(Fikentscher,Cellulosechemie 13,1932(58))により測定されるK値40を特徴とする溶液粘度を有するポリビニルピロリドンを有するポリビニルピロリドン。
実施例1
温度計、ガス取込管およびディーンスタークトラップを備えた4リットルのガラス反応器において、287.17gのDCDPS、203.89gのDHDPS、C16/C18部のモル比55:45および数平均分子量Mn3100g/モルを有する608.99gのα−C16/C18−アルキル,ω−ヒドロキシ−ポリエチレングリコール、ならびに体積平均粒度32.4μmを有する145.12gの炭酸カリウムを、窒素雰囲気中で527mlのNMP中に懸濁した。
温度計、ガス取込管およびディーンスタークトラップを備えた4リットルのガラス反応器において、287.17gのDCDPS、235.16gのDHDPS、C16/C18部のモル比55:45および数平均分子量Mn3100g/モルを有する236gのα−C16/C18−アルキル,ω−ヒドロキシ−ポリエチレングリコール、ならびに体積平均粒度32.4μmを有する145.12gの炭酸カリウムを、窒素雰囲気中で527mlのNMP中に懸濁した。
温度計、ガス取込管およびディーンスタークトラップを備えた4リットルのガラス反応器において、287.17gのDCDPS、225.15gのDHDPS、C16/C18部のモル比55:45および数平均分子量Mn3100g/モルを有する328.1gのα−C16/C18−アルキル,ω−ヒドロキシ−ポリエチレングリコール、ならびに体積平均粒度32.4μmを有する145.12gの炭酸カリウムを、窒素雰囲気中で527mlのNMP中に懸濁した。
温度計、ガス取込管およびディーンスタークトラップを備えた4リットルのガラス反応器において、287.19gのDCDPS、231.40gのDHDPS、数平均分子量Mn8000g/モルを有する320gのポリエチレングリコール、ならびに体積平均粒度32.4μmを有する145.12gの炭酸カリウムを、窒素雰囲気中で527mlのNMP中に懸濁した。
温度計、ガス取込管およびディーンスタークトラップを備えた4リットルのガラス反応器において、574.16gのDCDPS、485.33gのDHDPS、C16/C18部のモル比55:45および数平均分子量Mn3100g/モルを有する186gのα−C16/C18−アルキル,ω−ヒドロキシ−ポリエチレングリコール、ならびに体積平均粒度32.4μmを有する290.24gの炭酸カリウムを、窒素雰囲気中で527mlのNMP中に懸濁した。
磁気撹拌機を備えた三ツ口フラスコ中に、76mlのN−メチルピロリドン(NMP)、5gのポリビニルピロリドン(PVP、Luvitec(登録商標)K40)および19gのポリエーテルスルホン(PESU、Ultrason(登録商標)E 6020P)を添加した。ポリエーテルスルホンの一部を第2表に示される量でコポリマーCと置き換えることによって、第2表に示される組成を有する混合物を調製した。該混合物を、均質で澄明な粘性溶液が得られるまで60℃で優しく撹拌しながら加熱した。その溶液を、室温で一晩脱ガスした。その後に、膜溶液を60℃で2時間にわたり再加熱し、そしてガラス板上でキャスティングナイフ(300ミクロン)を用いて60℃で、5mm/分の速度で作動するErichsen社の塗工機を使用してキャスティングした。膜の塗膜を30秒間にわたり静置し、それから25℃の水浴中で10分間にわたり浸漬した。
直径60mmを有する圧力セルを使用して、膜の純水透過を、超純水(Millipore 限外濾過(UF)システムによって濾過された無塩水)を使用して試験した。後続の試験では、種々のPEG標準の溶液を、0.15barの圧力で濾過した。供給物と透過液のGPC測定によって、分子量カットオフを測定した。
M3CおよびM5Cによる試料を、膜M3およびM5と同様にして調製したが、コポリマーCを含む実施例1または2により得られた20mlの溶液を500mlのエタノールで処理することでコポリマーCを沈殿させることによって得られた固体形の沈殿したコポリマーC1およびC2を使用して調製した。こうして得られた沈殿物を、100mlのエタノールで3回洗浄し、そして40℃および20mbarで乾燥させた。得られたポリマーは、ワックス様であった。
Claims (8)
- 膜Mの製造方法であって、以下のステップ:
a)コポリマーCを製造するステップであって、該コポリマーCが、少なくとも1種のポリアリーレンエーテルAのブロックとポリアルキレンオキシドPAOのブロックとを含み、該コポリマーC中のポリアルキレンオキシドPAOの含有量が、30質量%〜90質量%であり、かつコポリマーCは、溶剤L中で製造されて、溶液Sが得られるステップ、
b)少なくとも1種のポリマーPを含むドープ溶液Dを準備するステップ、
c)溶液Sとドープ溶液Dとを混合するステップ、
d)その溶液Sとドープ溶液Dとの混合物を、少なくとも1種の凝固剤と接触させることによって膜を製造するステップ
を含み、前記少なくとも1種のポリアリーレンエーテルAのブロックは、ポリエーテルスルホン、ポリスルホンおよびポリフェニレンスルホンまたはそれらのコポリマーもしくは混合物から選択され、前記ポリマーPは、ポリエーテルスルホン、ポリスルホンおよびポリフェニレンスルホンから選択され、かつ、前記ポリアルキレンオキシドは、ポリエチレンオキシドである、製造方法。 - 前記溶剤Lは、NMPである、請求項1に記載の方法。
- 前記少なくとも1種の凝固剤は、水を含む、請求項1または2に記載の方法。
- 前記膜Mは、コポリマーCおよびポリマーPを、1:99〜1:3の質量比で含有する、請求項1から3までのいずれか1項に記載の方法。
- 前記ポリアルキレンオキシドPAOのブロックは、150g/モル〜20000g/モルの平均分子量Mnを有する、請求項1から3までのいずれか1項に記載の方法。
- 前記ドープ溶液Dは、ポリビニルピロリドン、ポリエチレンオキシドおよび/またはフェノキシ樹脂から選択される更なる添加剤を更に含む、請求項1から4までのいずれか1項に記載の方法。
- 前記コポリマーCは、芳香族ビスハロゲノ化合物および芳香族ビフェノールまたはそれらの塩を、少なくとも1種の塩基の存在下で、かつ少なくとも1種のポリアルキレンオキシドPAOの存在下で反応させることによって製造される、請求項1から5までのいずれか1項に記載の方法。
- 請求項1から7までのいずれか1項に記載の方法により得られる膜M、または膜Mを含む膜モジュール、濾過システムの、水処理用途、工業廃水もしくは都市廃水の処理、海水もしくは汽水の脱塩のための、透析、食品加工のための使用。
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US10441925B2 (en) | 2019-10-15 |
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