JPH0416217A - Evaluation of dividing performance of ultrafiltration membrane - Google Patents
Evaluation of dividing performance of ultrafiltration membraneInfo
- Publication number
- JPH0416217A JPH0416217A JP11653590A JP11653590A JPH0416217A JP H0416217 A JPH0416217 A JP H0416217A JP 11653590 A JP11653590 A JP 11653590A JP 11653590 A JP11653590 A JP 11653590A JP H0416217 A JPH0416217 A JP H0416217A
- Authority
- JP
- Japan
- Prior art keywords
- colloidal silica
- ultrafiltration membrane
- evaluation
- fractionation performance
- membrane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000012528 membrane Substances 0.000 title claims abstract description 28
- 238000000108 ultra-filtration Methods 0.000 title claims abstract description 14
- 238000011156 evaluation Methods 0.000 title abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000008119 colloidal silica Substances 0.000 claims abstract description 24
- 238000005194 fractionation Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 238000010008 shearing Methods 0.000 abstract 1
- 239000000725 suspension Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 239000002202 Polyethylene glycol Substances 0.000 description 10
- 229920001223 polyethylene glycol Polymers 0.000 description 10
- 239000000126 substance Substances 0.000 description 8
- 239000011550 stock solution Substances 0.000 description 7
- 102000004169 proteins and genes Human genes 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 3
- 239000012466 permeate Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229920002307 Dextran Polymers 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 102000034238 globular proteins Human genes 0.000 description 2
- 108091005896 globular proteins Proteins 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野]
本発明は、限外濾過膜の分画性能の設計、品質管理、仕
様説明等に用いるための分画性能評価方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for evaluating fractionation performance for use in designing, quality control, specification explanation, etc. of fractionation performance of an ultrafiltration membrane.
一般に、限外濾過膜の分画性能は、予めサイズのわかっ
ている指標物質を用い、これをクリーンな純水に溶かし
た溶液を膜濾過し、指標物質の阻止率を測定することに
よって評価されている。Generally, the fractionation performance of an ultrafiltration membrane is evaluated by using an indicator substance whose size is known in advance, dissolving it in clean pure water, filtering it through the membrane, and measuring the rejection rate of the indicator substance. ing.
ここで阻止率とは、 原液の溶質濃度−透過液の″溶質濃度 阻止率− (χ) 原液の溶質濃度 の意味である。Here, the inhibition rate is Solute concentration of stock solution - Solute concentration of permeate Rejection rate - (χ) Solute concentration of stock solution This is the meaning of
また分画分子量とは、ある分子量のわかっている指標物
質(例えば、分子量20.000のポリエチレングリコ
ール)を、90%阻止する膜を「ポリエチレングリコー
ル基準の分画分子量20.000 Jと呼ふ、分画性能
の表現方法のことである。Molecular weight cutoff refers to a membrane that blocks 90% of an indicator substance with a known molecular weight (for example, polyethylene glycol with a molecular weight of 20.000), which is called a molecular weight cutoff of 20.000 J based on polyethylene glycol. This is a method of expressing fractionation performance.
従来より分画性能評価に用いられる指標物質としては、
デキストランやポリエチレングリコール等の高分子、あ
るいは酵素等の球状タンパク質等が挙げられる。Indicator substances traditionally used for evaluation of fractionation performance include:
Examples include polymers such as dextran and polyethylene glycol, and globular proteins such as enzymes.
しかし、デキストランやポリエチレングリコール等の高
分子は鎖状形状であるため、圧力条件や流れ(膜面流速
)による剪断力条件が変化した場合、形状や向きが自由
に変化し、膜の透過しやすさが変化する。 従って膜の
分画性能評価における阻止率が上記条件の影響を大きく
受けるため、膜自体の真の分画性能を評価す・ることか
難しかった。However, since polymers such as dextran and polyethylene glycol have a chain shape, when the shear force conditions due to pressure conditions or flow (membrane surface flow velocity) change, the shape and orientation change freely, making it easier for them to permeate through the membrane. It changes. Therefore, the rejection rate in evaluating the fractionation performance of the membrane is greatly affected by the above conditions, making it difficult to evaluate the true fractionation performance of the membrane itself.
一方、酵素等のタンパク賞は、■非常に高価であるため
多量かつ頻繁に使用できない、■タンパク質同士の化学
的相互作用による結合の影響を避けるために、特定のp
Hでかつ電解質を含む溶媒を用いなければならない、■
タンパク質と膜材質問の化学的相互作用によって阻止率
が影響を受ける、■タンパク質の種類によって■、■の
性質か大きく異なる、■タンパク質が変形しやすいので
阻止率が圧力条件や流れによる剪断力条件の影響を受け
る、■ポンプ等で強く攪拌した場合、分解や変形を起こ
す、等の種々の問題を有するため、前記高分子物質以上
に取り扱いが難しい。On the other hand, proteins such as enzymes are: - extremely expensive and cannot be used in large quantities and frequently;
A solvent that is H and contains an electrolyte must be used, ■
The rejection rate is affected by the chemical interaction between the protein and the membrane material. ■The properties of ■ and ■ vary greatly depending on the type of protein. ■ Since the protein is easily deformed, the rejection rate depends on pressure conditions and shear force conditions due to flow. It is more difficult to handle than the above-mentioned polymeric substances because it has various problems such as 1) decomposition or deformation when strongly agitated with a pump or the like.
従って、かかる圧力条件、流れによる剪断力条件、その
他の化学的物理的な条件の影響を受けずに安定して分画
性能評価を行うことができる指標物質は今まで見いださ
れていなかった。Therefore, no indicator substance has been found so far that allows stable evaluation of fractionation performance without being affected by such pressure conditions, shear force conditions due to flow, and other chemical and physical conditions.
本発明では、コロイダルシリカ粒子を用いることにより
上記問題点を解決できることを見いだした。In the present invention, it has been discovered that the above problems can be solved by using colloidal silica particles.
即ち本発明は、コロイダルシリカ粒子を用いることを特
徴とする限外濾過膜の分画性能評価方法を提供する。That is, the present invention provides a method for evaluating the fractionation performance of an ultrafiltration membrane, which is characterized by using colloidal silica particles.
本発明におけるコロイダルシリカ粒子とは、無機珪酸の
超微粒子のことで、水を分散媒として無水珪酸の超微粒
子を水中に分散せしめてなるコロイド溶液である。 か
かるコロイダルシリカ粒子の平均粒子径は、1mμm〜
100mμmが好ましい。Colloidal silica particles in the present invention are ultrafine particles of inorganic silicic acid, and are a colloidal solution prepared by dispersing ultrafine particles of silicic anhydride in water using water as a dispersion medium. The average particle diameter of such colloidal silica particles is 1 mμm to
100 mμm is preferred.
かかるコロイダルシリカ粒子は、安価で入手しやす(、
安定した性質を有するので取り扱いも容易である。 ま
た、粒径分布範囲が狭いのでシャープな分画性能評価が
可能である。 市販のものとしては、例えば、日産化学
■製の商品名「スノーテックス」等を好適に用いること
ができるが、これに限定されるものではない。。Such colloidal silica particles are inexpensive and easily available (
It has stable properties and is easy to handle. Furthermore, since the particle size distribution range is narrow, sharp evaluation of fractionation performance is possible. As a commercially available product, for example, the product name "Snowtex" manufactured by Nissan Kagaku ■ can be suitably used, but it is not limited thereto. .
一般に、球状タンパク質の粒子径rと分子量M−との関
係は、一般に、
r(入)=2×〜ワ償(Ferryの式)で表される。In general, the relationship between the particle diameter r and the molecular weight M- of a globular protein is generally expressed as: r (in) = 2 x (Ferry's equation).
「スノーテックス」のコロイダルシリカ粒子の粒子サイ
ズには、粒径4〜61Iull、7〜9altII11
.10〜20 mμ1等があるため、上記式を用いれば
これらの分子量は、順に8,000〜27,000.4
3,000〜91,000.125,000〜1,00
0,000に相当する。The particle sizes of the colloidal silica particles of "Snowtex" include particle sizes of 4 to 61 Iull, 7 to 9 altII11
.. Since there are 10 to 20 mμ1, etc., using the above formula, the molecular weight of these is 8,000 to 27,000.4 in order.
3,000~91,000.125,000~1,00
Equivalent to 0,000.
また、コロイダルシリカ粒子の粒子径は、BET法(表
面吸着法の一種)によって測定することができる。Further, the particle diameter of colloidal silica particles can be measured by the BET method (a type of surface adsorption method).
コロイダルシリカ粒子の表面には、−5iOH基及び−
0H−イオンが存在し、アルカリイオンによって電気二
重層が形成され、粒子間の反発により安定化されている
。 この電荷バランスがくずれると、粒子同士が結合
し凝集がおこるため好ましくない。The surface of the colloidal silica particles contains -5iOH groups and -
0H- ions are present, an electric double layer is formed by alkali ions, and is stabilized by repulsion between particles. If this charge balance is disrupted, particles will bond with each other and aggregation will occur, which is not preferable.
コロイダルシリカ粒子のpHに対する影響は、pH10
,5以上で溶解し、pHが酸性域になると凝集しやすく
なる。 またコロイダルシリカ粒子濃度が高いほど凝集
しやすくなる。The influence of colloidal silica particles on pH is as follows: pH 10
, 5 or higher, and tends to aggregate when the pH is in the acidic range. Furthermore, the higher the concentration of colloidal silica particles, the more likely they are to aggregate.
本発明においては、かかるコロイダルシリカ粒子溶液(
市販の溶液濃度は20〜30重量%)を、純水で10〜
10,000ppm 、好ましくはioo〜2.000
ppmとなるように希釈し、塩酸及び水酸化ナトリウム
でpH6〜IO1好ましくはpH7〜9に調整して、限
外濾過膜の分画性能評価に用いる。In the present invention, such a colloidal silica particle solution (
The concentration of commercially available solutions is 20-30% by weight), and the concentration is 10-30% by weight with pure water.
10,000ppm, preferably ioo~2.000
ppm, adjusted to pH 6 to IO1, preferably pH 7 to 9, with hydrochloric acid and sodium hydroxide, and used for evaluating the fractionation performance of ultrafiltration membranes.
なお、原液及び透過液中に含まれるコロイダルシリカ濃
度の定量は、I CP (Inductively C
oupled Plasma Atomic Emis
sion Spectrometer)法あるいは蒸発
乾固法によって行うことができる。Note that the concentration of colloidal silica contained in the stock solution and permeate can be determined using I CP (Inductively C
Oupled Plasma Atomic Emis
This can be carried out by the ion spectrometer method or the evaporation to dryness method.
次に実施例により、本発明をより具体的に説明する。 Next, the present invention will be explained in more detail with reference to Examples.
限外濾過膜として、日東電工■製、中空糸状限外濾過膜
を使用した。 かかる分画分子量はポリエチレングリコ
ール基準で20,000 (タンパク質基準で6,00
0 )相当である。 この限外濾過膜をポリプロピレン
製チューブ内に注型し、長さ20CI11の膜モジュー
ルを作製した。As the ultrafiltration membrane, a hollow fiber ultrafiltration membrane manufactured by Nitto Denko ■ was used. The molecular weight fraction is 20,000 based on polyethylene glycol (6,000 based on protein).
0) Considerable. This ultrafiltration membrane was cast into a polypropylene tube to produce a membrane module with a length of 20 CI11.
評価用原液のコロイダルシリカ溶液には、日産化学株製
のスノーテックスXS(粒子径4〜6幀μm)を用い、
適宜クリーン水で希釈し、塩酸及び水酸化ナトリウムに
てpH調整を行い評価を行った。For the colloidal silica solution of the stock solution for evaluation, Snowtex XS (particle size 4 to 6 μm) manufactured by Nissan Chemical Co., Ltd. was used.
It was diluted with clean water as appropriate, and the pH was adjusted with hydrochloric acid and sodium hydroxide for evaluation.
阻止率は、セイコー電子工業■製プラズマ発光分析装置
5PS−7000を用い、IPC法にて原液及び透過液
のケイ素濃度を測定し、次式により算出して求めた。The rejection rate was determined by measuring the silicon concentration of the stock solution and the permeated solution by the IPC method using a plasma emission spectrometer 5PS-7000 manufactured by Seiko Electronics Co., Ltd. and calculating it using the following formula.
原液のケイ素濃度−透過液のケイ素濃度また、比較例で
用いたポリエチレングリコール(分子120,000)
については、クリーンな純水に溶解して評価原液とし、
阻止率は屈折計にて濃度を測定し求めた。Silicon concentration of stock solution - silicon concentration of permeated solution Also, polyethylene glycol used in comparative example (120,000 molecules)
For evaluation, dissolve it in clean pure water and use it as an evaluation stock solution.
The rejection rate was determined by measuring the concentration using a refractometer.
実施例1
コロイダルシリカ(平均粒径50人(換算分子量15.
000) )溶液を、濃度1.OOOppm、 pH8
に調整し、これを膜面線速0.6m/sec、平均圧力
0.5.1.0.1.5 kgf/cjの各条件で、膜
モジュールの内側より濾過させた時のコロイダルシリカ
粒子の阻止率を第1図に示す。Example 1 Colloidal silica (average particle size 50 (converted molecular weight 15.
000) ) solution at a concentration of 1. OOOppm, pH8
colloidal silica particles when filtered from the inside of the membrane module under the following conditions: membrane surface linear velocity of 0.6 m/sec, average pressure of 0.5, 1, 0, 1,5 kgf/cj Figure 1 shows the inhibition rate.
比較例1
ポリエチレングリコール(分子量20,000)溶液を
濃度5.0OOppa+に調整し、これを実施例1と同
様の条件下で濾過させた時のポリエチレングリコールの
阻止率を第1図に併せて示す。Comparative Example 1 A polyethylene glycol (molecular weight 20,000) solution was adjusted to a concentration of 5.0OOppa+ and filtered under the same conditions as in Example 1. The rejection rate of polyethylene glycol is also shown in Figure 1. .
実施例2
コロイダルシリカ(平均粒径50人(換算分子量15.
000) )溶液を、濃度1,000ppm、 pH8
に調整し、これを平均圧力1.0 kgf/cd、膜面
線速0.2.0.6.1 n+/secの各条件で、膜
モジュールの内側より濾過させた時のコロイダルシリカ
粒子の阻止率を第2図に示す。Example 2 Colloidal silica (average particle size 50 (converted molecular weight 15.
000) ) solution at a concentration of 1,000 ppm and a pH of 8.
of colloidal silica particles when filtered from inside the membrane module under the following conditions: average pressure 1.0 kgf/cd, membrane surface linear velocity 0.2. The rejection rate is shown in Figure 2.
比較例2
ポリエチレングリコール(分子量20,000)溶液を
濃度5.000ppn+に調整し、これを実施例2と同
様の条件下で濾過させた時のポリエチレングリコールの
阻止率を第2図に併せて示す。Comparative Example 2 A polyethylene glycol (molecular weight 20,000) solution was adjusted to a concentration of 5.000 ppn+ and filtered under the same conditions as in Example 2. The rejection rate of polyethylene glycol is also shown in Figure 2. .
実施例3
pH6,8,10の3種類のコロイダルシリカ(平均粒
径50人(換算分子量15,000) ) 1.000
ppm溶液を用い、平均圧力1.0 kgf/c1i1
.膜面線速0.6 m/secの条件で、膜モジュー
ルの内側より濾過させた時のコロイダルシリカ粒子の阻
止率を第3図に示す。Example 3 Three types of colloidal silica with pH 6, 8, and 10 (average particle size 50 (converted molecular weight 15,000)) 1.000
Using ppm solution, average pressure 1.0 kgf/c1i1
.. Figure 3 shows the rejection rate of colloidal silica particles when filtered from the inside of the membrane module under the condition of membrane surface linear velocity of 0.6 m/sec.
II 1 図
上記実施例より明らかな如く、限外濾過膜のコロイダル
シリカの阻止率は、圧力条件及び流れによる剪断力条件
の影響をほとんど受けなかった。II 1 Figure As is clear from the above example, the rejection rate of colloidal silica in the ultrafiltration membrane was hardly affected by pressure conditions and shear force conditions due to flow.
また、コロイダルシリカ溶液のpHに対しても、pH6
〜10の中性域ではほとんど影響を受けなかった。Also, the pH of the colloidal silica solution is 6.
There was almost no effect in the neutral range of ~10.
本発明によれば、圧力条件や流れによる剪断力条件の影
響をほとんど受けず、かつpH条件についても、pH6
〜10の中性域でほとんど影響を受けることなく、限外
濾過膜の分画性能評価を行うことができる。According to the present invention, it is almost unaffected by pressure conditions and shear force conditions due to flow, and also with respect to pH conditions, pH 6.
The fractionation performance of the ultrafiltration membrane can be evaluated with almost no influence in the neutral range of ~10.
第1〜3図は、実施例及び比較例で得られた阻止率の測
定結果を表すグラフである。
(以上)1 to 3 are graphs showing measurement results of rejection rates obtained in Examples and Comparative Examples. (that's all)
Claims (1)
限外濾過膜の分画性能評価方法。(1) A method for evaluating the fractionation performance of an ultrafiltration membrane characterized by using colloidal silica particles.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11653590A JP2851371B2 (en) | 1990-05-02 | 1990-05-02 | Ultrafiltration membrane fractionation performance evaluation method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11653590A JP2851371B2 (en) | 1990-05-02 | 1990-05-02 | Ultrafiltration membrane fractionation performance evaluation method |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH0416217A true JPH0416217A (en) | 1992-01-21 |
JP2851371B2 JP2851371B2 (en) | 1999-01-27 |
Family
ID=14689534
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP11653590A Expired - Lifetime JP2851371B2 (en) | 1990-05-02 | 1990-05-02 | Ultrafiltration membrane fractionation performance evaluation method |
Country Status (1)
Country | Link |
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JP (1) | JP2851371B2 (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006255673A (en) * | 2005-03-18 | 2006-09-28 | Kurita Water Ind Ltd | Membrane evaluation method in membrane separation apparatus |
JP2009011927A (en) * | 2007-07-04 | 2009-01-22 | Tokyo Institute Of Technology | Ultrafiltering membrane, manufacturing method of the same and method for sorting size of nano-particle |
JP2010017647A (en) * | 2008-07-10 | 2010-01-28 | Metawater Co Ltd | Method for inspecting membrane |
JP2010253334A (en) * | 2009-04-21 | 2010-11-11 | Sepa Sigma Inc | Aqueous solution with distributed ferric hydroxide colloidal particles for nondestructive membrane performance and integrity test, and method of manufacturing the aqueous solution |
-
1990
- 1990-05-02 JP JP11653590A patent/JP2851371B2/en not_active Expired - Lifetime
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006255673A (en) * | 2005-03-18 | 2006-09-28 | Kurita Water Ind Ltd | Membrane evaluation method in membrane separation apparatus |
JP2009011927A (en) * | 2007-07-04 | 2009-01-22 | Tokyo Institute Of Technology | Ultrafiltering membrane, manufacturing method of the same and method for sorting size of nano-particle |
JP2010017647A (en) * | 2008-07-10 | 2010-01-28 | Metawater Co Ltd | Method for inspecting membrane |
JP2010253334A (en) * | 2009-04-21 | 2010-11-11 | Sepa Sigma Inc | Aqueous solution with distributed ferric hydroxide colloidal particles for nondestructive membrane performance and integrity test, and method of manufacturing the aqueous solution |
Also Published As
Publication number | Publication date |
---|---|
JP2851371B2 (en) | 1999-01-27 |
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