CN1555288A - 过滤膜 - Google Patents
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Abstract
本发明涉及基于热塑性聚合物的具有新型多孔结构的多孔模制体，特别是膜，本发明还涉及制备这类模制体，特别是膜的方法。这类膜可用作过滤膜。
Description
本发明涉及一种基于热塑性聚合物的具有新型多孔结构的多孔模制体，特别是膜，本发明还涉及一种制备这类模制体，特别是膜的方法。这类膜可用作过滤膜。
从现有技术已知一类多孔模制体，特别是以膜的形式用于微过滤领域和粗过滤领域的流体过滤的模制体，如用于工业、实验室和环境保护领域中的液体介质的预过滤和滤除过滤。例如在WO 99/38604中描述了一种由热塑性聚合物构成的泡沫状多孔膜，它具有至少80％的高开孔性和至少75％的孔隙体积。该膜具有良好的过滤特性，但是还有一些参数如膜的选择性和流通量仍要按需求加以改进。
由此，本发明的目的在于提供一种新型多孔模制体，特别是过滤膜，该膜应具有非常高的流通量，同时具有高的选择性。
该目的是通过权利要求中的表明的实施方案实现的。特别是提供一种基于至少一种热塑性聚合物的多孔模制体，其特征在于，以包含至少部分是开口的孔的结构作为多孔主结构，以在孔壁上的孔作为多孔次结构。构成该多孔模制体的结构可以特别是泡沫结构。优选构成本发明这类模制体的泡沫结构中作为多孔主结构的孔的开孔性≥75％，孔隙体积≥85％，优选≥95％。本发明的模制体特别是可在微过滤领域和粗过滤领域中用于流体过滤的膜，如用于工业、实验室和环境保护领域中的预过滤和滤除过滤。
此外，本发明还涉及一种基于至少一种热塑性聚合物的具有泡沫结构的膜，该泡沫结构包含其开孔性≥75％的作为多孔主结构的孔和作为多孔次结构的在孔壁中的孔，并且孔隙体积≥85％，优选≥95％。构成多孔主结构的孔呈球形或多面体形，并且通过其壁厚优选为约10-7m的孔壁相互邻接。孔的大小通常可依制备条件调节，如下面所说明的。优选孔具有同样大小，其范围为1-200μm，优选30-200μm。该泡沫结构的孔密度与孔大小有关，在孔大小约200μm时，孔密度一般为约106个孔/cm3；在孔大小约1μm时，孔密度约1013个孔/cm3。在多孔主结构中，开孔的平均孔径的标准偏差优选为＜20％。
孔的孔壁不是密封的，而是有形成孔的穿孔，称为“多孔二次结构”。这些孔或网状的穿孔或网状开孔的孔径≤10μm，优选0.1μm-10μm。
在本发明范围内，对包含孔作为多孔主结构和在孔壁中的孔作为多孔次结构的本发明的结构，优选采用非晶形的和/或部分晶形的热塑性聚合物作为热塑性聚合物，选自聚烯烃如聚丙烯、聚酯、聚酰胺、聚砜、聚醚砜、聚苯乙烯、纤维素衍生物、其取代产物和其混合物。
本发明的膜可以是非增强的或一面增强的或两面增强的。特别是该增强材料例如一面或两面可带有本发明的膜或该增强材料可在一面或两面上增强本发明的膜。作为增强材料可采用由金属或聚合物材料制成的薄膜、织物、针织物或无纺织物。优选采用由与构成本发明膜的泡沫结构的聚合物或聚合物混合物属于同类聚合物的聚合物纤维组成的材料。在本发明的优选实施方案中，该聚合物纤维由第一种高熔点的和高强度的芯体聚合物组成，其表面完全或部分覆盖一层第二种聚合物。这类构成的膜形状特别稳定。第二种聚合物比第一种聚合物有较低的熔点，并是耐化学性的。优选它与构成本发明膜的泡沫结构的聚合物或聚合物混合物是同一类聚合物。
附图简介：
图1A和1B是按实施例1制备的由发泡聚丙烯制成的过滤膜截面的放大60倍(A)和200倍(B)的扫描电子显微镜照片。该样品是在液氮中经脆性断裂制备的。从(A)中可清楚地看到孔密度约为106个孔/cm3的具有100-200μm的同样孔大小的多孔主结构。在(B)中可看出基于孔壁的穿孔形成的多孔次结构。该孔的直径为约10μm数量级。
图2是放大10000倍的穿孔孔壁的扫描电子显微镜照片，在此样品中，网状开孔(“孔径”)为≤1μm数量级。
图3是按实施例2的本发明的泡沫结构的扫描电子显微镜照片。
在作为过滤膜应用时，在本发明的泡沫结构情况下，较大孔的基体的孔壁具有其直径小于大孔基体的孔直径的大量的网状穿孔或网状开孔，即“双结构”，这种泡沫结构出乎意料地表明有非常高的流通量，同时有高的选择性。与现有技术中已知的具有对称或非对称的海绵结构或销形结构相反，本发明膜的新型泡沫结构显示出泡沫孔大小间距的准串接的过滤面。由此与通常的三维海绵结构相反，其有效膜厚度和阻力变小。
孔隙体积％按(1-粗密度/聚合物密度)×100计算，用％表示。该粗密度定义为单位体积的泡沫质量，它通过合适样品的秤重和其线性尺寸计算的体积来确定。
开孔性，即开孔部分的含量，用％表示是采用空气比较比重计测定的。在此方法中，通过比较样品的几何体积和相同压力下的参比体积可得出通过泡沫物质的空气排出，即相应于包括泡沫物质的闭合孔的体积。由在表面上的切开的孔产生的误差通过测量不同表面/体积比的样品来校正。将所测定的开孔性外推到表面/体积比为零的点来确定开孔性。
孔的大小分布由润湿膜的空气流量与压力的关系曲线来测定，该膜的孔用市售的通常采用的孔填料充填。空气流量采用库乐尔特(Coulter)孔度计测量。
此外，本发明还涉及一种制备前述本发明模制体，特别是膜的方法，其中将包括气体和气体混合物的成孔剂加到在挤出设备中的由至少一种非晶形和/或部分晶形的聚合物组成的聚合物熔体中，将由聚合物熔体和成孔剂组成的混合物在混合设备中加工成单相或均匀的熔体，并在通过成型喷嘴后该成孔剂通过入射的压力降使单相熔体发泡以制得本发明的泡沫结构，成孔剂的加入量要使在单相熔体中溶解的气体或气体混合物的总浓度按所用聚合物计＞4重量％，并且单相熔体的加工温度低于聚合物熔体的加工温度。在本发明方法的优选实施方案中，气体或气体混合物含CO2和/或He。熔体的加工温度优选低于聚合物熔体的加工温度20-100℃。术语“加工温度”在这里意指各制造商建议不含成孔剂的纯聚合物的加工温度，在此温度下可保证挤出机的正常运行。
在WO 99/38604中描述了制备本发明模制体或膜的一般方法步骤以及挤出设备。特别是由至少一种非晶形或部分晶形的聚合物组成的聚合物熔体在压力(60-100bar)下通过单螺杆挤出机或双螺杆挤出机送入挤出设备。在挤出机的2/3处加入成孔剂。例如该成孔剂是由二氧化碳、氮、氦或另一种惰性气体组成的气体或气体混合物。注入到聚合物熔体中的成孔剂多于在注入位置的温度或压力情况下在聚合物熔体中按热力学可溶解的量，即气体或气体混合物呈过量存在。在挤出机的圆筒之后可选择性地利用冷却延长段，以提高挤出机的混合作用。接着将聚合物/气体混合物经齿轮泵送入附加的混合段中，例如静态混合器和热交换器中。该附加混合段是由在出口处的第二齿轮泵邻接。由此可在附加混合段形成与挤出压力无关的压力水平。该混合段的压力水平除与设备参数(各热交换管的直径、长度等)有关外，还与熔体的通过量和粘度有关。由此可将入口压力调到≥400bar，出口压力调到≥300bar，并且在利用熔体的软化效应下导致熔体例如以ΔT＝50℃，优选ΔT＝100℃冷却。这两种措施导致较高的气体溶解度，以使过量的气体量溶解。然后将均匀的聚合物/气体溶液或单相熔体通过第二齿轮泵送入喷嘴，并相应于喷嘴成形。在喷嘴的出口处，聚合物发泡以形成本发明的泡沫结构。孔的大小和孔的密度通过均匀溶解的气体浓度来确定。
通过下列实施例对本发明进行详述。
实施例1
挤出设备相应于WO 99/38604中描述的设备。聚丙烯(PP 3660，Fina公司)的颗粒通过温度为180℃的挤出机以6kg/h的通过量挤出。在170bar压力下经计量设备将气体，即按所用聚合物计4.1重量％的CO2引入。经齿轮泵将该聚合物/气体混合物送入混合设备中，调节其中的压力，此压力与挤出机中的压力无关。如此经齿轮泵的压力调节，以使在给定熔体温度约为175℃下其出口压力约为150bar。在混合设备中的停留时间约为15-20分钟。第二齿轮泵后面的压力约为155bar。
使用4.1重量％CO2和175℃熔体温度条件下，得到图1A和1B中所示的泡沫结构。该泡沫的孔大小约为150μm，孔密度为1×106个孔/cm3，孔隙体积＞95％。形成大量多孔次结构，结果产生非常高的孔隙率。
实施例2
相应于实施1进行，但是采用由5％CO2和0.65％氦组成的气体混合物。在熔体温度为175℃下产生图3所示的泡沫结构。该泡沫的孔大小约为150μm，孔密度为1×106个孔/cm3，孔隙体积＞95％。形成大量多孔次结构，结果产生非常高的孔隙率。
Claims (13)
1.基于至少一种热塑性聚合物的多孔模制体，其特征是具有一种结构，该结构包括作为多孔主结构的孔和作为多孔次结构的在孔壁中的孔。
2.权利要求1的模制体，其中所述结构是泡沫结构。
3.权利要求2的模制体，所述泡沫结构具有其开孔性≥75％和孔隙体积≥85％的作为多孔主结构的孔。
4.权利要求1-3之一的模制体，其呈膜的形式。
5.基于至少一种热塑性聚合物的具有泡沫结构的膜，其中泡沫结构包括其开孔性≥75％的作为多孔主结构的孔和作为次结构的在孔壁中的孔，并且其孔隙体积≥85％。
6.权利要求5的膜，其中多孔主结构中的孔径为30-200μm。
7.权利要求5或6的膜，其中多孔主结构中的平均孔径的标准偏差＜20％。
8.权利要求5-7之一的膜，其中多孔次结构中的孔径为≤10μm。
9.权利要求5-8之一的膜，其中热塑性聚合物选自聚烯烃、聚酯、聚酰胺、聚砜、聚醚砜、聚苯乙烯、纤维素衍生物、其取代产物和其混合物。
10.权利要求5-9之一的膜，该膜被单侧或两侧增强。
11.一种制备前述权利要求之一的多孔模制体，特别是膜的方法，其中将含气体或气体混合物的成孔剂加到挤出设备中的由至少一种非晶形和/或部分晶形的聚合物组成的聚合物熔体中，将该由聚合物熔体和成孔剂组成的混合物在混合设备中加工成单相熔体，并在通过成形喷嘴后成孔剂通过入射的压力降使单相熔体发泡以制得泡沫结构，其中成孔剂的加入量要使在单相熔体中溶解的气体或气体混合物的总浓度＞4重量％，并且单相熔体的加工温度低于聚合物熔体的加工温度。
12.权利要求11的方法，其中所述气体或气体混合物含CO2和/或He。
13.权利要求11或12的方法，其中单相熔体的加工温度为低于聚合物熔体的加工温度20-100℃。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10145968.8 | 2001-09-18 | ||
| DE10145968A DE10145968B4 (de) | 2001-09-18 | 2001-09-18 | Filtrationsmembran |
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| Publication Number | Publication Date |
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| CN1555288A true CN1555288A (zh) | 2004-12-15 |
| CN1243601C CN1243601C (zh) | 2006-03-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN02818205.7A Expired - Fee Related CN1243601C (zh) | 2001-09-18 | 2002-09-04 | 多孔过滤膜及其制备方法 |
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| Country | Link |
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| US (1) | US20040245172A1 (zh) |
| EP (1) | EP1427516B1 (zh) |
| CN (1) | CN1243601C (zh) |
| AT (1) | ATE457821T1 (zh) |
| DE (3) | DE10145968B4 (zh) |
| WO (1) | WO2003024576A2 (zh) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492999A (zh) * | 2011-12-21 | 2012-06-13 | 东南大学 | 一种可实现静电纺丝法量产纳米纤维的喷头 |
| CN103706259A (zh) * | 2014-01-09 | 2014-04-09 | 天津工业大学 | 一种多孔膜及其成孔方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8403557B2 (en) * | 2006-09-28 | 2013-03-26 | University Of Washington | Micromixer using integrated three-dimensional porous structure |
| US7763456B2 (en) * | 2006-09-28 | 2010-07-27 | University Of Washington | 3D micro-scale engineered tissue model systems |
| US8247464B2 (en) | 2006-09-28 | 2012-08-21 | University Of Washington | Method of selective foaming for porous polymeric material |
| CN101700447B (zh) * | 2009-10-29 | 2011-09-14 | 上海正永海绵制品有限公司 | 滤水泡棉及其生产方法 |
| DE102010038984B4 (de) | 2010-08-05 | 2021-08-26 | BSH Hausgeräte GmbH | Aufschäumvorrichtung |
| US20140339165A1 (en) * | 2013-05-14 | 2014-11-20 | Pall Corporation | High throughput membrane with rough surface |
| US20140339164A1 (en) * | 2013-05-14 | 2014-11-20 | Pall Corporation | High throughput membrane |
| US9808770B2 (en) * | 2013-05-14 | 2017-11-07 | Pall Corporation | High throughput membrane with channels |
| EP3100849B1 (en) * | 2016-03-04 | 2018-05-09 | Top Express Holding Limited | Composite textile and method of producing same |
| US11060215B2 (en) | 2017-01-26 | 2021-07-13 | Bright Cheers International Limited | Reinforced composite fabric and method for preparing the same |
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| US3549423A (en) * | 1967-06-30 | 1970-12-22 | Gen Electric | Method for manufacturing foam type electrode |
| US3939849A (en) * | 1970-11-18 | 1976-02-24 | Monsanto Chemicals Limited | Filter elements |
| GB1482216A (en) * | 1974-04-11 | 1977-08-10 | Monsanto Ltd | Cigarette filters |
| US4473665A (en) * | 1982-07-30 | 1984-09-25 | Massachusetts Institute Of Technology | Microcellular closed cell foams and their method of manufacture |
| US4904385A (en) * | 1985-05-23 | 1990-02-27 | The Dow Chemical Company | Porous filter media and membrane support means |
| EP0422251A4 (en) * | 1989-04-18 | 1992-02-26 | Daicel Chemical Industries, Ltd. | Method of producing modified porous membrane |
| US5061767A (en) * | 1990-10-05 | 1991-10-29 | State University Of New York | Hydrophilic-hydrophobic polymer composites and membranes |
| US5158986A (en) * | 1991-04-05 | 1992-10-27 | Massachusetts Institute Of Technology | Microcellular thermoplastic foamed with supercritical fluid |
| DE4437860A1 (de) * | 1994-10-22 | 1996-04-25 | Basf Ag | Verfahren zur Herstellung von mikrozellulären Schäumen |
| JP3493079B2 (ja) * | 1995-06-19 | 2004-02-03 | 東燃化学株式会社 | 熱可塑性樹脂微多孔膜の製造方法 |
| US6005013A (en) * | 1995-08-14 | 1999-12-21 | Massachusetts Institute Of Technology | Gear throttle as a nucleation device in a continuous microcellular extrusion system |
| DE19803362A1 (de) * | 1998-01-29 | 1999-08-05 | Sartorius Gmbh | Geschäumte poröse Membranen aus thermoplastischen Polymeren sowie Verfahren und Vorrichtung zu ihrer Herstellung |
| US6620356B1 (en) * | 2000-04-18 | 2003-09-16 | Integra Lifesciences Corp. | Porous constructs fabricated by gas induced phase inversion |
| US7087200B2 (en) * | 2001-06-22 | 2006-08-08 | The Regents Of The University Of Michigan | Controlled local/global and micro/macro-porous 3D plastic, polymer and ceramic/cement composite scaffold fabrication and applications thereof |
-
2001
- 2001-09-18 DE DE10145968A patent/DE10145968B4/de not_active Expired - Fee Related
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2002
- 2002-09-04 DE DE50214218T patent/DE50214218D1/de not_active Expired - Lifetime
- 2002-09-04 EP EP02779303A patent/EP1427516B1/de not_active Expired - Lifetime
- 2002-09-04 CN CN02818205.7A patent/CN1243601C/zh not_active Expired - Fee Related
- 2002-09-04 AT AT02779303T patent/ATE457821T1/de not_active IP Right Cessation
- 2002-09-04 US US10/490,564 patent/US20040245172A1/en not_active Abandoned
- 2002-09-04 WO PCT/EP2002/009904 patent/WO2003024576A2/de not_active Application Discontinuation
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492999A (zh) * | 2011-12-21 | 2012-06-13 | 东南大学 | 一种可实现静电纺丝法量产纳米纤维的喷头 |
| CN102492999B (zh) * | 2011-12-21 | 2014-07-09 | 东南大学 | 一种可实现静电纺丝法量产纳米纤维的喷头 |
| CN103706259A (zh) * | 2014-01-09 | 2014-04-09 | 天津工业大学 | 一种多孔膜及其成孔方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2003024576A3 (de) | 2003-09-12 |
| EP1427516B1 (de) | 2010-02-17 |
| DE10145968A1 (de) | 2003-04-10 |
| DE50214218D1 (de) | 2010-04-01 |
| CN1243601C (zh) | 2006-03-01 |
| ATE457821T1 (de) | 2010-03-15 |
| DE20213713U1 (de) | 2003-01-09 |
| EP1427516A2 (de) | 2004-06-16 |
| US20040245172A1 (en) | 2004-12-09 |
| WO2003024576A2 (de) | 2003-03-27 |
| DE10145968B4 (de) | 2004-04-15 |
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