WO1994009888A1 - Procede de microfiltration a ecoulement transversal - Google Patents

Procede de microfiltration a ecoulement transversal Download PDF

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Publication number
WO1994009888A1
WO1994009888A1 PCT/US1993/010303 US9310303W WO9409888A1 WO 1994009888 A1 WO1994009888 A1 WO 1994009888A1 US 9310303 W US9310303 W US 9310303W WO 9409888 A1 WO9409888 A1 WO 9409888A1
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WO
WIPO (PCT)
Prior art keywords
pressure
membrane
flow
permeate
cross
Prior art date
Application number
PCT/US1993/010303
Other languages
English (en)
Inventor
Kent B. Mcreynolds
Allyn R. Marsh, Iii
Original Assignee
The Dow Chemical Company
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 The Dow Chemical Company filed Critical The Dow Chemical Company
Priority to JP6511283A priority Critical patent/JPH08502923A/ja
Priority to EP93925076A priority patent/EP0666773A4/fr
Publication of WO1994009888A1 publication Critical patent/WO1994009888A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K11/00—Fructose
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/147—Microfiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/22—Controlling or regulating
    • 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
    • B01D65/08—Prevention of membrane fouling or of concentration polarisation
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/16—Purification of sugar juices by physical means, e.g. osmosis or filtration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
    • B01D2321/04—Backflushing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
    • B01D2321/20—By influencing the flow
    • B01D2321/2008—By influencing the flow statically
    • B01D2321/2025—Tangential inlet

Definitions

  • the present invention relates to cross-flow microfiltration for removal of suspended and colloided solids and/or emulsified oil from liquids, particularly from water, waste-water, industrial waste, and industrial process streams.
  • Comstock et al. recognizes the desirability of operating in a steady state with nearly constant flux rate when the driving pressure differential is held constant, but acknowledges its inability to achieve such conditions in practice. Since Comstock et al. was unable to solve this problem, it proposed a method of increasing the time-averaged cross-flow filtration flux of a liquid through a porous microfiltration medium by maintaining the filtration flux rate at a pre-selected substantially constant value during the entire filtration run by applying a variable throttling pressure on the filtrate side and reducing the throttling pressure during the run to control the instantaneous value of the pressure differential as required to maintain the pre-selected flux rate, the flux rate being greater than the equilibrium flux rate.
  • the present invention provides a further improvement in the art by providing a method of establishing such a steady state cross-flow filtration flux in a cross-flow membrane filtration system.
  • the essence of the invention is determining a maximum transmembrane pressure by an iterative process whereby the transmembrane pressure is maintained at an initially low rate at which the process is in steady state and gradually increased to the point where process parameters such as concentrate pressure or permeate pressure just begin to vary and is then decreased slightly to the steady state condition. The system is then maintained at this point.
  • the advantages of this process include steady state operation which permits prolonged system operation without the necessity of shutdown for backflushing and/or other cleaning and operating at the highest transmembrane pressure that permits steady state operation.
  • the filtration module employed in the method of this invention describes a flow length such that the permeate pressure is equal to the concentrate pressure, thus defining a maximum recovery per pass achievable during steady state operation.
  • the latter requires that there is no net fouling along the entire membrane length. That is, at any point, the rate of deposition of foulant caused by the permeate flow to the membrane surface is exactly opposed by the rate of foulant removal induced by tangential shear forces of the cross flowing stream. Implicit in the criteria of a maximum recovery per pass is the relationship that maximum steady state flux or permeate flow will increase with increasing cross-flow velocity.
  • a particular advantage of the present system is that by operating under the steady state conditions, it is possible for the system to operate for extended periods of time without the membrane becoming fouled to the extent that it is necessary to shut down the system to clean the membrane.
  • the system is commercially practical because it can be operated for days or weeks without the necessity of backflushing and/or other cleaning.
  • Figure 1 is a graph showing the feed, concentrate, and permeate pressures obtained in the steady state operation of this invention.
  • the process or method of this invention is independent of the filtration membrane or apparatus employed.
  • Filtration modules may be employed in any configuration, but are generally employed in series, parallel, or a combination of both, with parallel being generally employed, and oriented in any manner, but typically either horizontally or vertically.
  • Typical filtration membranes that may be employed in the practice of this invention include, for example, membranes described in U. S. Patent 4,798,847 issued January 17, 1989, to Roesink et al., incorporated herein by reference. Other useful membranes are described in U. S. Patent 5,076,925 issued December 31 , 1991, to Roesink et al. and U. S. Patent 5,096,585 issued
  • hydrophobic membranes that are modified for hydrophilic character by either blending or coating modifications.
  • Membranes may be tubular, capillary, flat sheet, hollow fiber, or spiral wound with capillary bore feed being generally preferred. It is desirable that the effective pore size of the membranes be in the range of from about 0.01 to about 10 microns, generally 0.1 to 1.0 microns, i.e., the mean flow pore diameters as defined by ASTM method F316-86 are from 0.01 to 10 microns.
  • Feed Pressure (P f ) is the pressure of the feed as it enters the filtration module; Concentrate is the portion of the feed that does not permeate through the membrane contained within the filtration module; Concentrate pressure (P c ) is pressure of the concentrate as it exits the filtration module;
  • Permeate pressure is pressure of the permeate as it is collected at the exterior of the tube
  • Transmembrane pressure is the pressure across the membrane contained within the filtration module and is 1/2(P f - P c ) - (Pp - P c ).
  • the present invention is a cross-flow microfiltration process in which steady state operation is obtained by an iterative process.
  • This process comprises beginning operation under conditions which result in a transmembrane pressure which is significantly lower than used in heretofore conventional systems. If rapid membrane fouling as shown by sharply decreasing permeate flow is observed, a lower TMP is used. Otherwise, the TMP is gradually increased to a point where process parameters begin to vary with time. At this point, the transmembrane pressure is decreased to a point at which process parameters are essentially constant and the system is maintained at essentially that transmembrane pressure.
  • transmembrane pressure Various techniques exist for controlling transmembrane pressure. In a preferred embodiment, this is accomplished by controlling the permeate pressure by, for example, use of a valve in the permeate line. Other techniques will be suitable as will be recognized by those skilled in the art.
  • the TMP is maintained such that the permeate pressure is equal to or greater than the concentrate pressure. It is preferred that the permeate pressure is maintained as close as equal to the concentrate pressure as possible. In some systems, such as process streams of raw beet juice or high fructose corn syrup, this means that for a single pass, recovery is maximized to a level no greater than about 6 percent.
  • steady state means that the various process parameters, including flux, concentrate pressure, permeate pressure, feed pressure, temperature, etc. remain relatively constant over an extended time period.
  • rate of membrane fouling is zero.
  • rate of deposition of foulant carried by the permeate flow to the membrane surface is opposed by the rate of foulant removal induced by tangential shear forces of the cross-flowing stream.
  • the steady state process of this invention permits the operation of a cross-flow microfiltration system for extended periods of time, i.e., days or weeks, without the need to stop the process for backflushing or other cleaning.
  • the present process obtains higher average flux rates.
  • the present invention is useful in treatment of various streams containing components to be separated by microfiltration.
  • streams include effluent steams from operations for the production of sugar such as raw beet effluent streams and high fructose corn syrup streams.
  • the process is useful in the treatment of waste streams from laundry applications such as exist in stone washing operations.
  • a microfiltration module (Film Tec part #90006, one square meter surface area, 0.2 micron pore size) is used to filter 30 percent dissolved solids dextrose solution containing 0.4 percent suspended solids (mainly proteinaceous) at a driving pressure differential of about 27.6 kPa, a single pass recovery rate of less than about 5 percent and a temperature of about 68°C Filtration is continued in an essentially steady state condition for several days with substantially no change in permeate flux rate.
  • the turbidity of the feed is about 150 NTU and the turbidity of the permeate is about 0.37 NTU (Nepholometer Turbidity Units) and the total yield of dextrose is greater than 90 percent.
  • a 30 percent dissolved solids saccharifi cation effluent containing 0.4 percent suspended solids is filtered employing a cross-flow microfiltration module having a polyethersulfone-polyvinyl pyrrolidone membrane having a pore size of 0.2 micron and a surface area of 1 square meter.
  • the feed flow rate is about 0.69 liters per second (yielding an average feed velocity of about 1.7 meters/second) and the flow direction is vertical.
  • the filtration is continued for about 14 days with the results being indicated in the following Table 1.
  • the initial feed turbidity in this experiment is about 108 NTU.
  • the permeate turbidity of all samples tested is 0.32 or less.
  • the purified yield of dextrose is greater than 99 percent without diafiltration.
  • a sample of unfiltered corn syrup containing 38 percent dissolved solids and 36 dextrose equivalents (DE) is treated.
  • the feed turbidity is 800 NTU (Nepholometer Turbidity Units) and is coarse filtered through a 600 micron filter prior to introduction into the cross flow microfiltration membrane system.
  • the membrane used is one having 10 square meter surface area and 0.2 micron pore size.
  • Table II the feed temperature varies from 175 to 185°F and the transmembrane pressure is at 34.83 kPa at the beginning of the run and is at 37.48 kPa at the end of the run.
  • Backflushing may be achieved by reversing feed and concentrate flow direction with or without the permeate valve closed. Increases in feed flow velocity during backflushing may be practiced but are generally unnecessary.
  • Other traditional types of backflushing for example, pumping permeate product back through the module, will also regenerate the membrane as will other traditional methods.
  • backflushing is necessary or desirable, the original flow rate is generally achieved unless the filter is biologically fouled. Backflushing may be carried out with water, if desirable.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

Procédé permettant d'établir un écoulement transversal de filtration à régime stable dans un module de filtration par membrane à écoulement transversal. Le procédé démarre à une pression membrane faible (TMP) et en un fonctionnement à régime stable, après quoi la TMP est augmentée de manière itérative jusqu'à ce que le fonctionnement commence à devenir instable. La TMP est alors légèrement réduite jusqu'à ce que le fonctionnement soit à nouveau stabilisé. Selon un mode préféré de réalisation on utilise un module de filtration, lequel présente un durée d'écoulement assurant au perméat une pression égale à celle du concentré.
PCT/US1993/010303 1992-10-30 1993-10-25 Procede de microfiltration a ecoulement transversal WO1994009888A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP6511283A JPH08502923A (ja) 1992-10-30 1993-10-25 交差流ミクロ濾過法
EP93925076A EP0666773A4 (fr) 1992-10-30 1993-10-25 Procede de microfiltration a ecoulement transversal.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US96964792A 1992-10-30 1992-10-30
US07/969,647 1992-10-30

Publications (1)

Publication Number Publication Date
WO1994009888A1 true WO1994009888A1 (fr) 1994-05-11

Family

ID=25515810

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US1993/010303 WO1994009888A1 (fr) 1992-10-30 1993-10-25 Procede de microfiltration a ecoulement transversal

Country Status (3)

Country Link
EP (1) EP0666773A4 (fr)
JP (1) JPH08502923A (fr)
WO (1) WO1994009888A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0747111A1 (fr) * 1995-05-08 1996-12-11 BUCHER-GUYER AG Maschinenfabrik Procédé pour augmenter la performance de filtration des filtres à courant transversal dans les modules des installations de filtration
NL1025717C2 (nl) * 2004-03-12 2005-09-13 Vitens Fryslon N V Werkwijze voor het zuiveren van een waterige stroom.
WO2015065795A1 (fr) * 2013-10-28 2015-05-07 Wincom, Inc. Purification de mélanges liquides contenant un composé hétéro-aromatique azole
DE102019101745A1 (de) * 2019-01-24 2020-07-30 Putsch Gmbh & Co. Kg Verfahren zum Betrieb einer Membranfilteranlage

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4751003A (en) * 1985-05-02 1988-06-14 Henkel Kommanditgesellschaft Auf Aktien Crossflow microfiltration process for the separation of biotechnologically produced materials
US4886602A (en) * 1987-09-15 1989-12-12 Henkel Kommanditgesellschaft Auf Aktien Process for the separation of biotechnologically produced valuable materials from a fermenter broth by crossflow micro- and/or ultrafiltration
US4906375A (en) * 1984-07-14 1990-03-06 Fresenius, Ag Asymmetrical microporous hollow fiber for hemodialysis
US5028436A (en) * 1987-12-21 1991-07-02 Gauri Kailash Kumar Membrane preparation and process for separating the dissolved and undissolved constituents of milk
US5047154A (en) * 1983-03-10 1991-09-10 C.P.C. Engineering Company Method and apparatus for enhancing the flux rate of cross-flow filtration systems

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT385426B (de) * 1986-06-30 1988-03-25 Vogelbusch Gmbh Verfahren zum kontinuierlichen filtrieren einer fluessigkeit und einrichtung zur durchfuehrung des verfahrens
JPS6397202A (ja) * 1986-10-15 1988-04-27 Toray Ind Inc ポリエ−テルスルホン系樹脂半透膜およびその製造方法
GB8923376D0 (en) * 1989-10-17 1989-12-06 Bio Flo Ltd Transmembrane pressure controlled filtration system

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5047154A (en) * 1983-03-10 1991-09-10 C.P.C. Engineering Company Method and apparatus for enhancing the flux rate of cross-flow filtration systems
US4906375A (en) * 1984-07-14 1990-03-06 Fresenius, Ag Asymmetrical microporous hollow fiber for hemodialysis
US4751003A (en) * 1985-05-02 1988-06-14 Henkel Kommanditgesellschaft Auf Aktien Crossflow microfiltration process for the separation of biotechnologically produced materials
US4886602A (en) * 1987-09-15 1989-12-12 Henkel Kommanditgesellschaft Auf Aktien Process for the separation of biotechnologically produced valuable materials from a fermenter broth by crossflow micro- and/or ultrafiltration
US5028436A (en) * 1987-12-21 1991-07-02 Gauri Kailash Kumar Membrane preparation and process for separating the dissolved and undissolved constituents of milk

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP0666773A4 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0747111A1 (fr) * 1995-05-08 1996-12-11 BUCHER-GUYER AG Maschinenfabrik Procédé pour augmenter la performance de filtration des filtres à courant transversal dans les modules des installations de filtration
NL1025717C2 (nl) * 2004-03-12 2005-09-13 Vitens Fryslon N V Werkwijze voor het zuiveren van een waterige stroom.
WO2015065795A1 (fr) * 2013-10-28 2015-05-07 Wincom, Inc. Purification de mélanges liquides contenant un composé hétéro-aromatique azole
US9309205B2 (en) 2013-10-28 2016-04-12 Wincom, Inc. Filtration process for purifying liquid azole heteroaromatic compound-containing mixtures
US9802905B2 (en) 2013-10-28 2017-10-31 Wincom, Inc. Filtration process for purifying liquid azole heteroaromatic compound-containing mixtures
DE102019101745A1 (de) * 2019-01-24 2020-07-30 Putsch Gmbh & Co. Kg Verfahren zum Betrieb einer Membranfilteranlage

Also Published As

Publication number Publication date
EP0666773A1 (fr) 1995-08-16
EP0666773A4 (fr) 1998-05-13
JPH08502923A (ja) 1996-04-02

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