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WO2008016292A1 - Membrane à fibre creuse céramique, module à membrane et processus de fabrication de la membrane - Google Patents

Membrane à fibre creuse céramique, module à membrane et processus de fabrication de la membrane Download PDF

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Publication number
WO2008016292A1
WO2008016292A1 PCT/NL2006/000354 NL2006000354W WO2008016292A1 WO 2008016292 A1 WO2008016292 A1 WO 2008016292A1 NL 2006000354 W NL2006000354 W NL 2006000354W WO 2008016292 A1 WO2008016292 A1 WO 2008016292A1
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WO
WIPO (PCT)
Prior art keywords
membranes
membrane
ceramic
hollow fibre
wall thickness
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.)
Ceased
Application number
PCT/NL2006/000354
Other languages
English (en)
Inventor
Rinse Alle Terpstra
Joost Petrus Gerardus Maria Van Eijk
Marcel Gerardus Cornelis Sars
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HYFLUX CEPARATION NV
Original Assignee
HYFLUX CEPARATION NV
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by HYFLUX CEPARATION NV filed Critical HYFLUX CEPARATION NV
Priority to PCT/NL2006/000354 priority Critical patent/WO2008016292A1/fr
Publication of WO2008016292A1 publication Critical patent/WO2008016292A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
    • C04B35/62286—Fibres based on nitrides
    • 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
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • 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
    • B01D69/08—Hollow fibre membranes
    • B01D69/087—Details relating to the spinning process
    • 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
    • B01D71/02—Inorganic material
    • B01D71/021—Carbon
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D71/0215—Silicon carbide; Silicon nitride; Silicon oxycarbide
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    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
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    • B01D71/025—Aluminium oxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D2325/00—Details relating to properties of membranes
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    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
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    • C04B2111/00801—Membranes; Diaphragms
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Definitions

  • the invention relates to a ceramic hollow fibre membrane for microfiltration, ultrafiltration and gas separation, having a porosity of at least 10%.
  • Membrane modules with ceramic hollow fibre membranes are for instance being employed in separation and concentration processes for separating and concentrating gasses and liquids.
  • Such a ceramic hollow fibre membrane is known from the international patent application with publication No. WO 94/23829. Because the surface area/volume ratio of this known fibre membrane is relatively high, the efficiency of the concentration or separation process will be high. In this document is noticed that the high surface area/volume ratio is of vital importance to be able to compete with other types of membranes.
  • These known hollow fibre membranes have an external diameter of 0,5-3 mm and a wall thickness of 30-500 micrometer. There is a constant development to increase the surface area/volume ratio in order to improve the efficiency.
  • An obj ective of the invention is to provide a ceramic hollow fibre membrane of the type described in the preamble of claim 1 with which a higher efficiency of the concentration or separation process will be possible than with the known fibre membrane.
  • the fibre membrane according to the invention is characterized in that said membrane has an external diameter of 3,1-10 mm and a wall thickness of 0,51-4,9 mm.
  • the existing direction of development is to increase the surface area/volume ratio in order to improve the efficiency
  • the present invention is based on the insight that a higher efficiency can be obtained with fibre membranes with a less surface area/volume ratio than that of the known fibre membranes.
  • the explanation for this is that hollow fibre membranes having a greater external diameter and a greater wall thickness are stronger and the separation or concentration processes can be carried out at higher pressures and higher flow rates which leads to a high increase in efficiency which is more than necessary to compensate the decrease in efficiency due to the lower surface area/volume ratio.
  • no higher pressures will be used less drop in pressure will occur, because the membranes according to the invention also have a greater internal diameter than the known membranes, and thus a lower pressure will be sufficient which results in a higher energetic efficiency.
  • the ceramic hollow fibre membrane has an external diameter of
  • An embodiment of the fibre membrane according to the invention is characterized in that on the inside and/or outside of the wall of the fibre membrane a thin ceramic coating is present. Preferably a ceramic coating is applied either on the inside or on the outside of the wall of the fibre membrane. Using such a fibre membrane the efficiency of a concentration or separation process can further be increased. When a substrate with large pores is used and a thin layer with the actual membrane pores is coated on that substrate the resistance of the flow is reduced which greatly enhances the flux.
  • the invention also relates to a membrane module comprising a bundle of ceramic hollow fibre membranes according to the invention, which membranes have a porosity of at least 10% and which membrane module has a flange on each end of the bundle fibre membranes.
  • the invention is characterized in that said membranes each have an external diameter of 3 ,5-4,5 mm and a wall thickness of 0,51 - 0,55 mm, preferably an external diameter of 3,5-4,5 mm and a wall thickness of 0,51-0,55 mm and more preferably an external diameter of 4 mm and a wall thickness of 0,52-0,54 mm.
  • An embodiment of the membrane module according to the invention is characterized in that said membranes each have an internal or external ceramic membrane coating.
  • the invention also relates to a method for producing a ceramic hollow fibre membranes for microfiltration, ultrafiltration and gas separation according to the invention, which membranes each have an external diameter of 3,1-10 mm and a wall thickness of 0,51-4,9 mm, said method comprising: making a paste by filling a thermoplastic polymer binder system with a ceramic powder; making said thermoplastic binder system plastic by heating; melt extruding the paste through a spinneret to produce ceramic hollow fibre membranes; heating the membranes to remove the binder system by thermal diffusion; and - sintering the powder particles to each other to obtain single layer hollow fibre membranes being free of an additional micro-porous layer, said fibre membranes having a porosity of at least 10%.
  • the invention is characterized in that a ceramic powder coating is applied on the inside and/or outside of the fibre membrane, and then the coating is dried and sintered.
  • a ceramic coating is applied either on the inside or on the outside of the fibre membrane.
  • An embodiment of the method according to the invention is characterized in that to remove the binder system the membranes are placed in a burn-off furnace in which hot air is circulated. Due to this circulation of hot air the process of removing the binder system is improved which results is a stronger membrane of a higher quality.
  • the binder used is a thermoplastic binder with the tradename Licomont from the firm Clariant.
  • an extruder 1 can be seen, which introduces the paste to be spun into three spinnerets 3 by means of a spinning pump 2.
  • the spinnerets 3 produce three continuous fibres.
  • the hollow fibres are cut at desired lengths at a cutting station 4.
  • the fibres 5 are laid against each other on a heating plate 6 in a furnace 7 to keep the fibres at a constant temperature of about 50 degrees Celsius to remove internal stresses.
  • the fibres 5 are placed in a burn-off furnace 8 in which hot air is circulated by means of a fan 9 to remove the binder system.
  • the fibres 5 are laid down and stacked in a sintering installation 10 in which they are sintered.
  • a ceramic powder coating is applied either on the inside or outside of the fibre membrane, and then the coating is dried and sintered.
  • the thickness of the coating layer can be between 10 nanometer and 5000 nanometer and the material of the coating is typically aluminium oxide (alumina), but can also be other type of ceramics/inorganic materials, including gamma alumina, titania, zirconia, silica, zeolite, carbon, microporous carbon, amorphous carbon, etc. and mixtures thereof.
  • the paste which is spun to give hollow fibre membranes consists of a thermoplastic polymer binder system and a ceramic powder.
  • the thermoplastic polymer system becomes plastic at a temperature of between 50 and 220 degrees Celsius and serves as an aid during shaping (and sintering).
  • the percentage of ceramic powder is between 30 and 70% V/V, preferably between 45 and 55% V/V.
  • the paste is mixed in a mixer and granulated after cooling.
  • the granules are then introduced into the extruder 1, where they melt again and, via the spinning pump 2 and spinnerets 3 are formed into hollow fibre membranes.
  • the polymer binder system is removed in the burn-off furnace 8, after which the residual shape is sintered in a sintering installation 10.
  • the thermoplastic binder in the paste is preferably a binder from the firm Clariant available under the tradename Licomont.
  • the ceramic powder in the paste preferably consists of aluminium oxide, although silicon nitride (Si 3 N 4 ), silicon carbide, sialon and other ceramic powders can also be used.
  • a certain amount of sinter aid for example itrium oxide or aluminium oxide, can be added to the paste to control the porosity.
  • the temperature in the burn-off furnace is about 500 degrees Celsius and that in the sintering furnace is about 1300 degrees Celsius in the case of aluminium oxide powder and about 1650 degrees Celsius in the case of silicon nitride powder. Sintering takes about 2 hours.
  • the hollow fibre membranes obtained are able to withstand a corrosive environment and a relatively high temperature.
  • the external diameter is preferably about 4 mm and the wall thickness is preferably between 0,52-0,54 mm.
  • the porosity is 30 to 50%.
  • Silicon nitride in particular has a high strength and density and, moreover, a very high temperature resistance and corrosion resistance.
  • the pore size can be adjusted between 0,02 and 3 micrometer and the density and the pore size can be controlled with the aid of the sinter aid and with the aid of the sintering temperature.
  • the ceramic powder chosen can also be hydroxyapatite, a ceramic powder that is biocompatible and that is used in artificial ossicles or as bone-replacement material.
  • the particle size distribution of the powder can be important. A broad distribution leads to a higher degree of filling.
  • the absolute particle size is important for the binder system removal process. The smaller the particles, the smaller will be the pores of the product formed and the more difficult it will be to remove the binder system. By adding relatively large amounts of sinter additives and/or by using a higher sintering temperature and longer sintering time, it should be possible to dense-sinter the hollow fibres produced by means of the invention.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

La membrane à fibre creuse céramique selon l'invention présente un diamètre externe d'environ 4 mm, une épaisseur de paroi de 0,52-0,54 mm, et est pourvue d'un mince revêtement céramique à l'intérieur ou à l'extérieur de la membrane à fibre. Dans un procédé de fabrication de ces membranes à fibre creuse, une pâte est injectée dans trois filières (3), qui produisent trois fibres continues qui sont découpées à des longueurs désirées. Ensuite, on dispose les fibres (5) les unes contre les autres sur une plaque de chauffage (6) dans un four (7) pour supprimer les contraintes internes, après quoi on place les fibres (5) dans un four de calcination (8) dans lequel on fait circuler de l'air chaud, afin de supprimer le système liant. L'étape suivante consiste à disposer et à empiler, les fibres (5) dans une installation de frittage (10) dans laquelle elles sont frittées. On applique ensuite un revêtement de poudre céramique à l'intérieur ou à l'extérieur de la membrane à fibre, puis le revêtement est séché et fritté.
PCT/NL2006/000354 2006-08-01 2006-08-01 Membrane à fibre creuse céramique, module à membrane et processus de fabrication de la membrane Ceased WO2008016292A1 (fr)

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RU2432986C1 (ru) * 2010-02-26 2011-11-10 Закрытое Акционерное Общество "Новомет-Пермь" Способ изготовления мембранного модуля
WO2014207140A1 (fr) 2013-06-27 2014-12-31 Mann+Hummel Gmbh Milieu céramique de filtre de sang total à membrane à fibres creuses et son utilisation pour la séparation de plasma/sérum sanguin à partir de sang total
WO2015014624A1 (fr) * 2013-07-31 2015-02-05 Mann+Hummel Gmbh Membranes de céramique à fibres creuses présentant des propriétés mécaniques améliorées
WO2015180954A1 (fr) * 2014-05-27 2015-12-03 Mann+Hummel Gmbh Membrane de filtration multicouche en céramique, notamment sous forme d'une fibre creuse
EP3404003A1 (fr) * 2017-05-17 2018-11-21 Vysoké Uceni Technické V Brne Procédé de production de fibres céramiques creuses ultra minces autoportantes par l'utilisation de gabarits sacrificiels

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WO1999022852A1 (fr) * 1997-11-05 1999-05-14 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Procede de production de membranes fibreuses creuses de microfiltration, ultrafiltration ou de separation de gaz
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GB2022565A (en) * 1978-05-16 1979-12-19 Monsanto Co Hollow fibres
JPS5959233A (ja) * 1982-09-28 1984-04-05 Mitsui Kensaku Toishi Kk 菌体ろ過用セラミツク中空糸体
WO1999022852A1 (fr) * 1997-11-05 1999-05-14 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Procede de production de membranes fibreuses creuses de microfiltration, ultrafiltration ou de separation de gaz
WO2002074421A1 (fr) * 2001-03-16 2002-09-26 The Robert Gordon University Appareil et procede de separation de gaz

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2432986C1 (ru) * 2010-02-26 2011-11-10 Закрытое Акционерное Общество "Новомет-Пермь" Способ изготовления мембранного модуля
AU2014301062B2 (en) * 2013-06-27 2018-11-15 Mann+Hummel Gmbh Ceramic whole blood hollow fiber membrane filter medium and use thereof for separating blood plasma / serum from whole blood
WO2014207140A1 (fr) 2013-06-27 2014-12-31 Mann+Hummel Gmbh Milieu céramique de filtre de sang total à membrane à fibres creuses et son utilisation pour la séparation de plasma/sérum sanguin à partir de sang total
DE102013010735A1 (de) 2013-06-27 2015-01-15 Mann + Hummel Gmbh Keramisches Vollbluthohlfasermembranfiltermedium und Verwendung davon zum Abtrennen von Blutplasma/-serum von Vollblut
US10500328B2 (en) 2013-06-27 2019-12-10 Mann+Hummel Gmbh Ceramic whole blood hollow fiber membrane filter medium and use thereof for separating blood plasma/serum from whole blood
US20190015791A1 (en) * 2013-07-31 2019-01-17 Mann+Hummel Gmbh Ceramic hollow fiber membranes with improved mechanical properties
CN105408009A (zh) * 2013-07-31 2016-03-16 曼·胡默尔有限公司 具有改善的机械特性的陶瓷空心纤维膜
CN105408009B (zh) * 2013-07-31 2018-01-16 曼·胡默尔有限公司 具有改善的机械特性的陶瓷空心纤维膜
US10029214B2 (en) 2013-07-31 2018-07-24 Mann+Hummel Gmbh Ceramic hollow fibre membranes with improved mechanical properties
CN108452686A (zh) * 2013-07-31 2018-08-28 曼·胡默尔有限公司 具有改善的机械特性的陶瓷空心纤维膜
WO2015014624A1 (fr) * 2013-07-31 2015-02-05 Mann+Hummel Gmbh Membranes de céramique à fibres creuses présentant des propriétés mécaniques améliorées
US10857505B2 (en) * 2013-07-31 2020-12-08 Mann+Hummel Gmbh Ceramic hollow fiber membranes with improved mechanical properties
DE102014007665A1 (de) * 2014-05-27 2015-12-17 Mann + Hummel Gmbh Filtermembran, Hohlfaser und Filtermodul
WO2015180954A1 (fr) * 2014-05-27 2015-12-03 Mann+Hummel Gmbh Membrane de filtration multicouche en céramique, notamment sous forme d'une fibre creuse
US10413870B2 (en) 2014-05-27 2019-09-17 Mann+Hummel Gmbh Ceramic multilayer filter membrane
EP3404003A1 (fr) * 2017-05-17 2018-11-21 Vysoké Uceni Technické V Brne Procédé de production de fibres céramiques creuses ultra minces autoportantes par l'utilisation de gabarits sacrificiels

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