EP2964366A1 - Procédé de filtration d'homopolysaccharides - Google Patents

Procédé de filtration d'homopolysaccharides

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Publication number
EP2964366A1
EP2964366A1 EP14708523.7A EP14708523A EP2964366A1 EP 2964366 A1 EP2964366 A1 EP 2964366A1 EP 14708523 A EP14708523 A EP 14708523A EP 2964366 A1 EP2964366 A1 EP 2964366A1
Authority
EP
European Patent Office
Prior art keywords
membrane
range
glucans
filtration
symmetrical
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
EP14708523.7A
Other languages
German (de)
English (en)
Inventor
Jörg Therre
Hartwig Voss
Tobias KÄPPLER
Sascha ROLLIE
Stephan Freyer
Bernd Leonhardt
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.)
BASF SE
Original Assignee
Wintershall Holding GmbH
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 Wintershall Holding GmbH filed Critical Wintershall Holding GmbH
Priority to EP14708523.7A priority Critical patent/EP2964366A1/fr
Publication of EP2964366A1 publication Critical patent/EP2964366A1/fr
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
    • 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
    • B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/06—Tubular membrane modules
    • 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
    • B01D69/04—Tubular membranes
    • B01D69/043—Tubular membranes characterised by the tube diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2317/00—Membrane module arrangements within a plant or an apparatus
    • B01D2317/02—Elements in series
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2317/00—Membrane module arrangements within a plant or an apparatus
    • B01D2317/06—Use of membrane modules of the same kind

Definitions

  • the present invention relates to an improved process for the filtration of aqueous fermentation broths containing glucans and biomass using symmetrical tubular membranes.
  • a deposit In natural oil deposits, petroleum is present in the cavities of porous reservoirs, which are closed to the earth's surface of impermeable cover layers.
  • the cavities may be very fine cavities, capillaries, pores or the like. Fine pore necks, for example, have a diameter of only about 1 ⁇ .
  • a deposit In addition to crude oil, including natural gas, a deposit contains more or less saline water.
  • polysaccharides from glucose are also called glucans.
  • the said branched homopolysaccharides have a
  • Homopolysaccharides of the named structure are secreted by various fungal strains, for example by the filamantos growing Basidiomycet Schizophyllum commune, which precipitates during growth a homopolysaccharide of said structure having a typical molecular weight Mw of about 2 to about 25 * 10 6 g / mol (common name Schizophyllan). Also to be mentioned are secreted by Sclerotium rolfsii
  • Homopolysaccharides of said structure (common name: scleroglucans).
  • EP 271 907 A2 and EP 504 673 A1 disclose methods of fungal strains for producing branched homopolysaccharides from ⁇ -1,3-linked glucose units.
  • the preparation is carried out by discontinuous fermentation of the strains with stirring and aeration.
  • the nutrient medium consists essentially of glucose, yeast extract, potassium dihydrogen phosphate, magnesium sulfate and water.
  • the polymer is secreted by the fungus into the aqueous fermentation broth and finally an aqueous polymer solution is separated from the biomass-containing fermentation broth, for example by centrifugation or filtration.
  • Schizophyllans is recommended for centrifugation and cross-flow microfiltration (supra, p. 78, para. 10.1).
  • cross-flow microfiltration there is the use of sintered stainless steel membranes with a pore size of 10 ⁇ the company Krebsoege (called today GKN) proposed.
  • WO 2003/016545 A2 discloses a continuous process for the preparation of
  • Scleroglucans using Sclerotium rolfsii for cleaning is a Cross-flow filtration using stainless steel filters of a pore size of 20 ⁇ described at an overflow velocity of at least 7 m / s.
  • WO 201 1/082973 A2 describes the cell separation by means of asymmetric membranes wherein the pore size of the separating layer is 1 ⁇ to 10 ⁇ .
  • Flat membranes or asymmetrical tubular membranes, single-channel modules or multi-channel modules can be used.
  • Fermentation broths are not suitable because the pore size is too small to allow schizophyllan to pass through the pores.
  • GIT suction garzeitung Labor (12/92 pages 1233 - 1238) describes the continuous production of branched glucans with cell recycling. This arrangement is also referred to in the literature as a membrane bioreactor with an external membrane stage. To separate the branched glucans from the fermentation cycle, a cross-flow filtration by means of stainless steel membranes is first proposed, which have a pore size of 200 ⁇ . As a further method for the second purification stage, the authors have unsuccessfully the
  • Fermentation broths can not be operated economically on an industrial scale.
  • Fermentation broths containing biomass and glucans in which a fermentation broth with a high average flow is passed through symmetrical tubular membranes, without the quality of the resulting aqueous solution of glucan is adversely affected, for example in the form of a higher content of cell fracture components.
  • a high average flux indicates that the process of separating glucans from fermentation broths containing biomass and glucan can be operated at a pumping rate that makes the process economical.
  • the above object has been achieved by the provision of a method for separating an aqueous solution of glucans from an aqueous fermentation broth containing glucans and biomass in a filtration plant, wherein symmetrical tubular membranes which are cylindrically shaped and a
  • the present invention therefore relates, in one embodiment, to a process for the separation of an aqueous solution of glucans from an aqueous one
  • Fermentation broth containing glucans and biomass in a filtration plant comprising at least the following steps
  • the symmetrical tube membrane having an inner diameter in the range> 2 mm and 6 mm and a degree of separation in the range of> 0.5 and 45 ⁇ , determined in accordance with ASTM F 795.
  • tubular membranes Symmetrical tubular membranes are called tubular membranes, the one
  • Symmetrical pipe membranes are known in the art and are described inter alia in T. Melin and R. Rautenbach, membrane process (basics of modular and system design), 3rd edition (2007), Springer Verlag, page 20 et seq.
  • a symmetrical tubular membrane which is cylindrically shaped, is a tubular membrane which extends along a longitudinal axis and has a cavity surrounded by walls, which has both a substantially polygonal and a round, i.e., a circular shape.
  • circular or oval may have cross section.
  • FIG. 2 Schematic representation of a filtration plant
  • Figure 3 Representation of a membrane element with hexagonal shaped body
  • FIG. 4 Schematic representation of a filtration plant
  • Glucans are a class of homopolysaccharides whose
  • Monomer component is exclusively glucose.
  • the glucose molecule can be linked in an ⁇ -glycosidic or ⁇ -glycosidic manner, branched out in different degrees or arranged linearly.
  • glucans are selected from the group consisting of cellulose, amylose, dextra n, glycogen, lichenin, laminarin from algae, pachyman from tree fungi and
  • Yeast glucans with ß-1,3-bond Nigeran, mycodextran isolated from fungi ( ⁇ -1,3-glucan, ⁇ -1,4-glucan), curdlan ( ⁇ -1,3-D-glucan), pullulan ( ⁇ -1, 4-linked and 1, 6-linked D-glucan) and schizophyllan ( ⁇ -1, 3-base chain, ⁇ -1, 6-side chain) and pustulan ( ⁇ -1, 6-glucan).
  • the glucan preferably comprises a main chain of ⁇ -1,3-glycosidically linked
  • the side groups consist of a single ß-1, 6 Glycosidically linked glucose unit, which, statistically speaking, every third unit of the main chain is linked to another glucose unit ⁇ -1, 6-glycosidically.
  • Schizophyllan has a structure according to formula (I) wherein n is a number in the range of 2500 to 35,000.
  • the fungal strains are selected from the group consisting of
  • Suitable fungal strains are furthermore mentioned, for example, in EP 271 907 A2 and EP 504 673 A1, in each case claim 1. Particularly preferably, the fungal strains used are
  • This fungal strain secretes a glucan, in which a
  • glucan Main chain of ß-1, 3-glycosidically linked glucose units-statistically seen every third unit of the main chain with another glucose unit ß-1, 6-linked glycose; i.e.
  • the glucan is the so-called
  • Typical schizophyllans have a weight average molecular weight Mw of about 2 to about 25.10 6 g / mol.
  • the fungal strains are fermented in a suitable aqueous medium or nutrient medium.
  • the fungi secrete the above class of glucans into the aqueous medium during fermentation.
  • the fermentation broth is obtained by mixing mushrooms in a suitable aqueous
  • Fermented medium The fungi secrete the above class of glucans into the aqueous fermentation broth during fermentation.
  • fungi may preferably be used in an aqueous nutrient medium, for example
  • the fermentations are driven so that the concentration of the glucans to be produced in the fermentation broth to be filtered is at least 8 g / l.
  • Upper limit is not limited in principle. It results from which viscosity is still manageable with the fermentation apparatus used in each case.
  • the fermentation is in a
  • suitable plant comprising at least one fermentation tank
  • the system is powered by a sidestream constantly or temporarily
  • Concentration than previously, also referred to as retentate, at least in part can be returned to the fermentation tank.
  • the present invention relates to a process for the separation of an aqueous solution of glucans comprising a backbone of ⁇ -1,3-glycosidically linked glucose units and ⁇ -1,6-glycosidically linked side groups from glucose units thereof aqueous Fermentation broth containing glucans comprising a backbone of ⁇ -1, 3-glycosidically linked glucose units and ⁇ -1, 6-glycosidically attached side groups of glucose units, and biomass in a filtration system comprising at least the following steps
  • the symmetrical tube membrane has an inner diameter in the range> 2 mm and ⁇ 6 mm.
  • the present invention relates to a process for the separation of an aqueous solution of glucans having a main chain of ⁇ -1, 3-glycosidically linked glucose units and ⁇ -1, 6-glycose
  • glucose groups comprising attached side groups from an aqueous fermentation broth containing glucans comprising a backbone of ⁇ -1, 3-glycosidically linked glucose units and ⁇ -1, 6-glycosidically linked side groups of glucose units and biomass in a filtration system comprising at least the following steps
  • the symmetrical tube membrane having an inside diameter in the range> 2 mm and 6 mm and a degree of separation in the range of> 0.5 and 45 ⁇ , determined according to ASTM F 795.
  • the tube membrane preferably the symmetrical tube membrane, a
  • Inner diameter as illustrated by the dimension A in Fig. 1, in the range> 3 mm and ⁇ 6 mm, particularly preferably in the range> 2 mm and ⁇ 5 mm and most preferably in the range> 2 mm and ⁇ 4 mm.
  • the tube membrane preferably the symmetrical tube membrane, pores having a pore size d90 in the range> 4 ⁇ and ⁇ 45 ⁇ , particularly preferably the
  • Pipe membrane preferably the symmetrical pipe membrane, pores with a pore size d90 in the range> 4 ⁇ and ⁇ 20 ⁇ , particularly preferably, the pipe membrane, preferably the symmetric pipe membrane, pores having a pore size d90 in the range> 4 ⁇ and ⁇ 9 ⁇ , each determined according to ISO 15901 -1.
  • pore size d90 is known to the person skilled in the art and is determined from a pore size distribution curve of the support material, the "pore size d90" designating that pore size at which 90% of the pore size
  • Pore volume of the material have a pore size ⁇ P orenhold d90.
  • Pore size distribution of a material can be determined, for example, by means of mercury porosimetry and / or gas adsorption methods.
  • the tubular membrane preferably the symmetrical tubular membrane, is preferably made of a material having a degree of separation in the range of> 0.5 and 45 ⁇ , particularly preferably in the range of> 1, 0 and 10 ⁇ , very particularly preferably in the range of > 1, 0 and -i 6.0 ⁇ , and in particular in the range of> 1, 0 and ⁇ 5,0 ⁇ , each determined in accordance with ASTM F 795.
  • the tube membrane preferably the symmetrical tube membrane, a length, as illustrated by the dimension C in Fig. 1, in the range> 0.2 m and ⁇ 1, 5 m, more preferably in the range> 0.2 m and ⁇ 1, 2 m, very particularly preferably in the range of 0.3 m and ⁇ 1.0 m and even more preferably in the range of> 0.3 m and 0.7 m.
  • the tube membrane preferably the symmetrical tube membrane, a
  • Wall thickness as indicated by the dimension B in Fig. 1, in the range> 0.3 mm and ⁇ 3.0 mm, particularly preferably in the range of> 1, 0 mm and ⁇ 2.0 mm. It is advantageous if a tube membrane is selected with the smallest possible wall thickness, since in this embodiment, a higher mean flow compared to a tube membrane with the same outer diameter and higher wall thickness can be achieved.
  • the tube membrane preferably the symmetrical tube membrane, a
  • the tube membranes used according to the invention are configured symmetrically.
  • the tube membranes may preferably be metallic tube membranes or ceramic tube membranes.
  • the tube membranes used preferably the symmetrical tube membranes used, are sintered metal tube membranes, preferably symmetrical sintered metal tube membranes.
  • the tube membranes used are sintered metal tube membranes, preferably symmetrical sintered metal tube membranes.
  • Sintered metal tubular membranes preferably the symmetrical sintered metal tubular membranes, of a material selected from the group consisting of stainless steel, titanium, nickel-copper alloy, nickel-chromium alloy, nickel-iron alloy, nickel-iron-chromium alloy, Bronze and zirconium.
  • These tube membranes are available, for example, from GKN Sinter Metals Filters GmbH, Radevormwald, Germany.
  • the cross section of the tube membrane preferably the symmetrical tube membrane, round.
  • the tube membranes preferably the symmetrical tube membranes, are preferably used as so-called mono channel elements.
  • the at least one tube membrane preferably the at least one, preferably forms
  • Tube membrane arranged, a membrane module.
  • the tube membranes can also be used as multi-channel elements.
  • the carrier material forms a shaped body, for example, a round or hexagonal shaped body, as shown by the designation D in Fig. 3, in the channels, as shown by the designation E in Fig. 3, are recessed.
  • the outer diameter of such a shaped body for a membrane module is preferably 5 mm to 100 mm, more preferably 10 mm to 50 mm.
  • the multi-channel elements offer the advantage of larger membrane area with the same space requirements and easier installation. The disadvantage is the compared to the
  • membrane modules may be arranged in parallel or in series in series.
  • Membrane modules arranged one behind the other in series.
  • cross-flow filtration also called cross-flow filtration
  • a flow of the liquid to be filtered is applied parallel to the surface of the membrane used as filtration material, for example by means of a suitable circulating pump.
  • the filter membrane is thus constantly flowed over by a liquid flow, and thereby the formation of deposits on the membrane surface is prevented or at least reduced.
  • all pump types are suitable as pumps. Because of the high viscosity of the fermentation broth, however, positive displacement pumps and especially eccentric screw pumps and rotary piston pumps have proven particularly suitable. Also suitable are centrifugal pumps, channel wheel pumps and pitot pumps.
  • the pipe membranes according to the invention are installed in suitable filter systems.
  • Constructions of suitable filter systems are known in principle to the person skilled in the art.
  • Tubular membranes preferably symmetrical tubular membranes, are used for carrying out the process according to the invention.
  • the retentate is preferably passed through the interior of the channel or channels, and the permeate occurs accordingly outward through the walls of the substrate in the
  • the feed stream is conducted in step b) with an overflow velocity in the range> 0.5 m / s and ⁇ 5 m / s, particularly preferably in the range> 2 m / s and ⁇ 4 m / s.
  • Too low a flow rate is unfavorable because the membrane then clogs quickly, too high a flow rate causes unnecessarily high costs because of the large amount of retentate to be circulated.
  • the temperature at which the feed stream is passed through the at least one tube membrane, preferably the at least one symmetrical tube membrane, is not critical and is preferably between 5 ° C and 150 ° C, preferably between 10 ° C and 80 ° C and most preferably between 15 ° C and 40 ° C. If the separated cells are not to be killed, for example in processes with recycling of the biomass, the temperature should be between 15 ° C and 40 ° C for a while.
  • the preferred apparatus comprises a
  • Circulation pump P1 a filter module F1 and a heat exchanger W1.
  • the pump P1 the abovementioned transverse flow of the liquid is produced over the surface of the tube membrane arranged in the filter apparatus F1.
  • a heat exchanger W1 the system contents can be tempered.
  • Several such filtration systems can be arranged in series or in parallel.
  • the filter apparatus F1 consists of a housing in which at least one tube membrane is introduced. Through the tube membrane, the housing is in a so-called
  • the liquid coming from the pump P1 is the fermentation broth containing biomass and glucan.
  • the feed enters the retentate space via at least one feed.
  • a liquid flow, called concentrate again from the
  • the pressure in the retentate space is higher than the pressure in the permeate space.
  • the pressure difference is called transmembrane pressure.
  • Part of the feed stream passes through the membrane and collects in the permeate space. This passing through part of the liquid, called permeate, represents the separated from biomass glucan solution.
  • the removal of the permeate stream and the retentate stream is carried out continuously, wherein the ratio of the amount of the permeate stream to the amount of the retentate stream is preferably in the range between 0.5 to 20.
  • the transmembrane pressure is preferably 0.1 bar to 1 0 bar, more preferably 0.5 bar to 6 bar, and very particularly preferably 1 bar to 4 bar.
  • the transmembrane pressure is preferably adjusted by bringing the transmembrane pressure in a ramp with a slope preferably between 0.05 bar / h and 2 bar / h to the desired value.
  • the operating time of the membrane filtration plant can optionally be replaced by a regular
  • Backwashing with permeate can be extended.
  • a pressure is applied at regular intervals in the permeate space, which is higher than the pressure in the retentate and for a defined time back a certain amount of permeate pushed back through the membrane in the retentate.
  • This backwashing can, for example, by pressing the permeate space with nitrogen, through a backwash pump or by using a piston system done as it eg under the name
  • the backwashing should be carried out at intervals of 5 minutes to 30 minutes, without the invention being limited to this time cycle.
  • the amount of backwashed permeate is preferably in the range of 0.1 to 5 l / m 2 membrane area, particularly preferably in the range of 0.1 to 2 l / m 2 membrane area.
  • the backwashing pressure is preferably in the range between 1 bar and 10 bar.
  • Cleaning solution at a temperature of from 20 ° C to 100 ° C, more preferably from 40 ° C to 80 ° C treated.
  • acids As a cleaning solution, acids
  • the acid concentration is preferably at a concentration of 1% by weight to 10% by weight. better
  • the concentration of leaches used is preferably between 0.1% by weight and 20% by weight.
  • oxidizing substances such as hydrogen peroxide, hypochlorite, in particular sodium hypochlorite or peracetic acid
  • the concentration of oxidizing substances should be 0.5% by weight to 10% by weight, in particular 1% by weight to 5% by weight.
  • the purification can be carried out with a mixture of hydrogen peroxide and alkali or hydrogen peroxide and hypochlorite.
  • the membranes are cleaned - with the system off - preferably in the installed state in the membrane filtration plant using a cleaning-in-place system (ClP system).
  • the inventive method is characterized in that the cleaning of the tube membranes must be made only when a permeate amount of more than 2000 kg / m 2 membrane area has been obtained. Thus, that allows inventive method long operating times, since the cleaning of the tube membranes can be done at long intervals.
  • a solution of glucans having a ⁇ -1,3-glycosidically linked main chain and ⁇ -1,6-glycosidically attached side groups suitable for tertiary mineral oil production can be prepared in a simple manner which has a concentration of the glucans in the range> 3 g / l and ⁇ 30 g / l, more preferably in the range> 3 g / l and ⁇ 20 g / l, most preferably> 5 g / l and ⁇ 15 g / l.
  • the yield of schizophyllan ie the amount of schizophyllan that can be recovered after filtration based on the amount of schizophyllan in the fermentation broth to be filtered, is preferably between 60% and 80%, more preferably between 65% and 75%.
  • the cross-flow filtration apparatus used is shown in FIG. It consisted of a stirred storage tank B1 with a volume of 4 liters, one
  • Circular piston pump P1 the tube heat exchanger W1, the pressure holding valve V1 and the filter module F1.
  • Cross-flow filtration system tempered to 30 ° C.
  • the filter module was a
  • the length of the membrane tube was 430 mm, the inner diameter was 3 mm and that was 6 mm.
  • Membrane area of the symmetrical tube membrane was 0.00368 m 2 .
  • the wall thickness of the symmetrical tube membrane was 1 .5 mm and the degree of separation, determined according to ASTM F 795, was 3 ⁇ m.
  • the filter module F1 was by means of valves V3 and V2 with permeate in
  • Example 2 The same cross-flow filtration apparatus and the same fermentation broth as in Example 1 were used. 1500 g of the fermentation broth was poured into the container B1 and with a
  • Circulation rate of 75 l / h circulated by the pump P1.
  • the overflow velocity was 2.9 m / s.
  • the transmembrane pressure was 0.8 bar, within 2 h, the transmembrane pressure was increased to 3 bar and for the remaining
  • the permeate was collected and weighed. By means of a state control, fermentation broth was refilled into the container during the filtration so that the content of the B1 was always kept at 1500 g. The filtration was operated for 63 h and collected during this time 10,500 g of permeate. The mean flow up to this time of filtration was 43.4 kg / h / m 2 . The collected permeate was analyzed and a glucan content of 6.7 grams per liter found, the filtration yield was thus 74%.
  • the retentate outgassing was operated at a ratio of produced permeate to discharged retentate equal to 7 to 1.
  • the plant was operated for another 30 hours.
  • 14204 g of permeate and 2032 g of retentate were produced.
  • the mean flow during the entire filtration was 41.5 kg / h / m 2 .
  • Filter load was over 3800 kg / m 2 .
  • the permeate was completely clear and contained no cell debris.
  • Circulation rate of 75 l / h circulated by the pump P1.
  • the overflow velocity was 2.9 m / s.
  • the transmembrane pressure was 0.8 bar, within 4 h, the transmembrane pressure was increased to 3 bar and for the remaining
  • the permeate was collected and weighed. By A level control was added during the filtration fermentation broth in the container so that the contents of B1 was always kept at 1500 g. The filtration was operated for 30 hours and collected during this time 10,500 g of permeate. The mean flow up to this time of filtration was thus 94.7 kg / h / m 2 . The collected permeate was analyzed and a glucan content of 6.2 grams per liter found, the filtration yield was thus 68%. Then the retentate outgassing with a ratio of
  • permeate to discharged retentate equal to 7 to 1 put into operation.
  • the system was operated for another 25 h.
  • 18,284 g of permeate and 2613 g of retentate were produced.
  • the mean flow during the entire filtration was 90.2 kg / h / m 2 .
  • the filter load was over 2600 kg / m 2 .
  • the permeate was completely clear and contained no cell debris.
  • Example 4 The same cross-flow filtration apparatus and the same fermentation broth as in Example 1 were used.
  • the overflow velocity was 2.9 m / s.
  • the transmembrane pressure was 0.8 bar, within 8 h, the transmembrane pressure was increased to 3 bar and for the remaining
  • the permeate was collected and weighed. By means of a state control, fermentation broth was refilled into the container during the filtration so that the content of the B1 was always kept at 1500 g. The filtration was operated for 37 hours and collected during this time 10,500 g of permeate. The mean flow up to this time of filtration was thus 77.4 kg / h / m 2 . The collected permeate was analyzed and a glucan content of 6.3 grams per liter found, the filtration yield was thus 68%. Then the retentate outgassing with a ratio of
  • Example 2 The same cross-flow filtration apparatus and the same fermentation broth as in Example 1 were used. 1500 g of the fermentation broth was poured into the container B1 and with a
  • the cross-flow filtration apparatus used is shown in FIG. 4. It consisted of a stirred double-jacket storage tank B1 with a volume of 120 liters, the eccentric screw pump P1, the tube bundle heat exchanger W1, the pressure-holding valve V1 and the filter module F1.
  • the filter modules F1 were called by means of a B3
  • Backwash apparatus BF100 of the company Pall back at intervals of 900 s each with 100 ml of permeate at a pressure of 10 bar backwashed.
  • the content of the cross-flow filtration system was cooled to 25 ° C. via the double jacket of the container B1 and the heat exchanger W1.
  • the filter module F1 seven symmetrical tubular membranes from GKN Sinter Metals Filters GmbH, Radevormwald, Germany, type SIKA R3 were used.
  • Membrane tubes were 1000 mm, the inner diameter was 6 mm and the outer diameter was 10 mm.
  • the usable membrane area of the symmetrical tubular membranes was 0.132 m 2 .
  • the wall thickness of the symmetrical tube membrane was 2 mm and the degree of separation, determined according to ASTM F 795, was 3 ⁇ .
  • the circulation rate of the pump P1 was set to 2.6 m 3 / h and a
  • the overflow velocity was 3.6 m / s.
  • the transmembrane pressure was increased slowly and after 18 hours was 1.5 bar.
  • Transmembrane pressure was held at this level for the remainder of the experiment.
  • the permeate was collected and weighed.
  • fermentation broth was refilled into the container during the filtration so that the contents of the B1 were always kept at 50 kg.
  • the filtration was operated for 71 hours and 230.8 kg of permeate was collected during this time.
  • the mean flow during filtration was 24.7 kg / h / m 2 .
  • the filter load was 1748 kg / m 2 .
  • the collected permeate was analyzed and a glucan content of 5.3 grams per liter found, the filtration yield was thus 57%.
  • the permeate was completely clear and contained no cell debris.

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  • Wood Science & Technology (AREA)
  • Sustainable Development (AREA)
  • Biotechnology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • Genetics & Genomics (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Apparatus Associated With Microorganisms And Enzymes (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

La présente invention se rapporte à un procédé amélioré de filtration de bouillons de fermentation aqueux contenant des glucanes et de la biomasse, ledit procédé comprenant l'utilisation de membranes tubulaires symétriques.
EP14708523.7A 2013-03-05 2014-02-26 Procédé de filtration d'homopolysaccharides Ceased EP2964366A1 (fr)

Priority Applications (1)

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EP14708523.7A EP2964366A1 (fr) 2013-03-05 2014-02-26 Procédé de filtration d'homopolysaccharides

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US201361772569P 2013-03-05 2013-03-05
EP13157826 2013-03-05
PCT/EP2014/053747 WO2014135417A1 (fr) 2013-03-05 2014-02-26 Procédé de filtration d'homopolysaccharides
EP14708523.7A EP2964366A1 (fr) 2013-03-05 2014-02-26 Procédé de filtration d'homopolysaccharides

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EP2964366A1 true EP2964366A1 (fr) 2016-01-13

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US (1) US20160002363A1 (fr)
EP (1) EP2964366A1 (fr)
CN (1) CN105008026B (fr)
CA (1) CA2898253A1 (fr)
RU (1) RU2656157C2 (fr)
WO (1) WO2014135417A1 (fr)

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WO2016087521A1 (fr) 2014-12-04 2016-06-09 Wintershall Holding GmbH Procédé de préparation d'une solution aqueuse de bêta-glucane
MX2019011647A (es) * 2017-03-28 2019-12-19 Cargill Inc Beta-glucanos refinados y métodos para elaborarlos.
EP3549958A1 (fr) * 2018-04-04 2019-10-09 Clariant International Ltd Procédé de purification de biocompositions complexes

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US6013185A (en) * 1997-09-25 2000-01-11 Rhodia Inc. Recovery and reuse of nonionic surfactants from aqueous solutions
JP2002112800A (ja) * 2000-10-04 2002-04-16 Kurita Water Ind Ltd デンプン糖化液精製装置
US7820194B2 (en) * 2001-12-21 2010-10-26 Alcon, Inc. Combinations of viscoelastics for use during surgery
RU2271675C1 (ru) * 2004-09-06 2006-03-20 Сергей Юрьевич Беглов Способ получения пектина
CN100422347C (zh) * 2006-02-07 2008-10-01 三达膜科技（厦门）有限公司 基于全膜法的结晶葡萄糖制造方法
FR2945043B1 (fr) * 2009-04-30 2019-07-26 Roquette Freres Procede de purification de polymeres de glucose destines aux solutions de dialyse peritoneale
ES2596656T3 (es) * 2009-12-17 2017-01-11 Wintershall Holding GmbH Procedimiento para la preparación de homopolisacáridos
CN102586361B (zh) * 2011-12-31 2014-04-09 三达膜科技（厦门）有限公司 一种葡萄糖的制造方法

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UDO RAU ED - VANDAMME ET AL: "Schizophyllan", 1 January 2002, BIOPOLYMERS / POLYSACCHARIDES II: POLYSACCHARIDES FROM EUKARYOTES, VERLAG WILEY-VCH, NEW YORK, US, PAGE(S) 63 - 79, ISBN: 978-3-527-30227-7, XP009512242 *
UDO RAU: "Passage", 1 January 1997, BIOSYNTHESE, PRODUKTION UND EIGENSCHAFTEN VON EXTRAZELLULÄREN PILZ-GLUCANEN, HABILITATIONSSCHRIFT, TECHNISCHE UNIVERSITÄT BRAUNSCHWEIG, SHAKER, DE, PAGE(S) 70 - 95, ISBN: 978-3-8265-2929-0, XP009512244 *

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RU2015141944A (ru) 2017-04-07
US20160002363A1 (en) 2016-01-07
CN105008026B (zh) 2017-12-22
WO2014135417A1 (fr) 2014-09-12
CA2898253A1 (fr) 2014-09-12
CN105008026A (zh) 2015-10-28
RU2656157C2 (ru) 2018-05-31

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