WO2019115772A1 - Adsorbent comprising metal dioxide and a polymeric material - Google Patents

Adsorbent comprising metal dioxide and a polymeric material Download PDF

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Publication number
WO2019115772A1
WO2019115772A1 PCT/EP2018/084969 EP2018084969W WO2019115772A1 WO 2019115772 A1 WO2019115772 A1 WO 2019115772A1 EP 2018084969 W EP2018084969 W EP 2018084969W WO 2019115772 A1 WO2019115772 A1 WO 2019115772A1
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WIPO (PCT)
Prior art keywords
porous
particulate material
present
polymeric material
particulate
Prior art date
Application number
PCT/EP2018/084969
Other languages
French (fr)
Inventor
Ernst MEINJOHANNS
Kenneth Harlow
Original Assignee
Upfront Chromatography A/S
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Filing date
Publication date
Application filed by Upfront Chromatography A/S filed Critical Upfront Chromatography A/S
Publication of WO2019115772A1 publication Critical patent/WO2019115772A1/en

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/282—Porous sorbents
    • B01J20/285—Porous sorbents based on polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/286—Phases chemically bonded to a substrate, e.g. to silica or to polymers
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00—Milk preparations; Milk powder or milk powder preparations
    • A23C9/14—Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009—Magnetic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3242—Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
    • B01J20/3268—Macromolecular compounds
    • B01J20/3272—Polymers obtained by reactions otherwise than involving only carbon to carbon unsaturated bonds
    • B01J20/3274—Proteins, nucleic acids, polysaccharides, antibodies or antigens
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3291—Characterised by the shape of the carrier, the coating or the obtained coated product
    • B01J20/3293—Coatings on a core, the core being particle or fiber shaped, e.g. encapsulated particles, coated fibers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/18—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
    • B01D15/1807—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns using counter-currents, e.g. fluidised beds

Definitions

  • the present invention relates to a novel particulate material .
  • the present invention relates to a novel particulate material comprising titanium dioxide for use as an adsorbent in downstream processing of liquid mixtures.
  • particulate materials have been used for years in processes of purifying compounds from complex medias like fermentation broths, plant extracts, and body fluids like blood and milk. There is a continuing need a demand from the industry to provide new particulate materials as the presently provided particulate materials may different disadvantages like leaking of particulate material, stability, functionality, addition of several undesirable components either coupled on the particulate material or used during the production of the particulate material .
  • an object of the present invention relates to a new particulate material .
  • one aspect of the invention relates to a particulate material comprising a particle comprising a non-porous material surrounded by a porous polymeric material, wherein the non-porous material comprises a titanium dioxide (TiCh) .
  • Another aspect of the present invention relates to a method of producing a particulate material, said method comprises the steps of:
  • step (ii) Heating the porous polymeric material suspension of step (i) to a
  • Yet another aspect of the present invention relates to the use of the particulate material according to anyone of claims 1-18 as an adsorbent for isolating one or more compounds from a liquid mixture.
  • the particulate material according to the present invention may preferably be suitable for isolating compounds from fermentation broths, plant extracts, and milk.
  • the liquid mixture may be a primary dairy source.
  • primary dairy source relates to a diary source comprising one or more milk oligosaccharides.
  • the primary diary source may preferably comprise one or more milk oligosaccharides and casein.
  • the dairy source may be selected from the group consisting of milk, whole milk, skimmed milk, milk concentrates, reconstituted milk powder, non-pasteurised milk, micro-filtrated milk, pH-adjusted milk, pre-treated dairy source, whey or a fraction obtained from whey.
  • a characteristic feature of the preliminary dairy source may be that the preliminary dairy source has not been subjected to casein precipitation, removal of casein micelles, and/or removal of the casein aggregates, prior to the separation of one or more oligosaccharide compound(s).
  • the preliminary dairy source may be obtained as the flow through obtained from a process of separating one or more milk proteins, such as the isolation process of isolation of soluble proteins from aggregated casein-containing mixtures, as described in WO
  • a particulate material comprising a particle comprising a non-porous material surrounded by a porous polymeric material, wherein the non-porous material comprises a titanium dioxide (T1O2).
  • non-porous material relates to a material that does not allow a liquid mixture to diffuse inside the material.
  • porous polymeric material relates to a material that allows a liquid mixture to diffuse inside the material.
  • the titanium dioxide present in the particulate material may have different forms and structures.
  • the particulate material comprises multiple titanium dioxide grains.
  • the titanium dioxide grain may have a mean grain size in the range of 10-100 nm, such as in the range of 12-75 nm, e.g. in the range of 15-50 nm, such as in the range of 18-30 nm, e.g. about 21 nm.
  • the multiple titanium dioxide grains, or the multiple non-porous grains, may be held together by the porous polymeric material.
  • the porous polymeric material may be an organic porous polymeric material.
  • the porous polymeric material or the organic porous polymeric material may be selected from agarose, alginate, chitosan, carrageenan, and/or pectin.
  • the organic porous polymeric material is agarose.
  • the particulate material may comprise a further non-porous material.
  • the particulate material may comprise a further non-porous material in addition to the titanium dioxide.
  • the term "further non-porous material” relates to a non-porous material different from titanium dioxide which may be included into the particulate material, resulting in a particulate material having at least two different types of non- porous materials.
  • the further non-porous material may be selected from a high density non-porous material; a silicate; a ceramic metal; alumina; or a magnetic material.
  • a high density non-porous material a silicate
  • a ceramic metal alumina
  • a magnetic material a material that is a sporous inorganic material.
  • non-porous core materials are described in WO 2010/037736, which is hereby incorporated by reference.
  • the high density non-porous material has a density of at least 4.0 g/ml, such as at least 10 g/ml, e.g. at least 16 g/ml, such as at least 25 g/ml.
  • the non-porous core material has a density in the range of about 4.0-25 g/ml, such as about 4.0-20 g/ml, e.g. about 4.0-16 g/ml, such as 12-19 g/ml, e.g. 14-18 g/ml, such as about 6.0-15.0 g/ml, e.g. about 6.0-16 g/ml.
  • the high density non-porous material may be tungsten carbide or steel or a combination hereof.
  • the non-porous material may constitute at least 10% (w/w), of the particulate material, such as at least 20% (w/w), e.g. at least 30%, such as at least 40% (w/w), e.g. at least 50%, such as at least 55% (w/w), e.g. at least 60%, such as at least 65% (w/w), e.g. at least 70%.
  • the content of titanium dioxide may preferably constitute at least 10% (w/w), of the particulate material, such as at least 20% (w/w), e.g. at least 30%, such as at least 40% (w/w), e.g. at least 50%, such as at least 55% (w/w), e.g. at least 60%, such as at least 65% (w/w), e.g. at least 70%.
  • the porous polymeric material may constitute at least 30% (w/w), of the particulate material, such as at least 40% (w/w), e.g. at least 50%, such as at least 55% (w/w), e.g. at least 60%, such as at least 65% (w/w), e.g. at least 70%, such as at least 80% (w/w), e.g. at least 90%.
  • the density of the adsorbent according to the present invention relates to the density of an adsorbent in it's fully solvated (e.g. hydrated) state as opposed to the density of a dried adsorbent particle.
  • the desired density of the one or more adsorbent may be provided by inclusion of a certain proportion or a certain amount of the non-porous material in the porous polymeric material.
  • the particulate material may have a density of at least 1.1 g/ml, more preferably at least 1.3 g/ml, still more preferably at least 1.5 g/ml, even more preferably at least 1.8 g/ml, even more preferably at least 2.0 g/ml, even more preferably at least 2.3 g/ml, even more preferably at least 2.5 g/ml, even more preferably at least 2.75 g/ml, even more preferably at least 3.0 g/ml, even more preferably at least 3.5 g/ml, even more preferably at least 4.0 g/ml.
  • At least 95% of the particulate material is substantially spherical.
  • the particulate material may be an adsorbent or part of an adsorbent material.
  • a ligand is coupled to the particulate material when using the particulate material as an adsorbent, e.g. in isolating compounds from complex medias like fermentation broths, plant extracts, and body fluids like blood and milk, however, titanium dioxide as used as non-porous material according to the present invention, may preferably as a ligand for isolating compounds from complex medias, or liquid media.
  • the one or more compounds to be isolated from the liquid mixture may preferably be one or more oligosaccharide compound.
  • the one or more oligosaccharide compound(s) comprises at least one moiety selected from the group consisting of a sialic acid moiety; Hexose moiety (a Hex moiety); a HexNAc moiety; and a NeuAc moiety.
  • the one or more oligosaccharide compound(s) comprises at least one moiety selected from a sialic acid moiety or a NeuAc moiety as the terminal moiety of the oligosaccharide.
  • the adsorbent comprising a ligand.
  • the non-porous material of the adsorbent, the titanium dioxide is acting as the ligand.
  • the particulate material according to the present invention may preferably be used as a chromatographic support.
  • the chromatographic support may be a membrane
  • the column chromatography support includes a Packed Bed Chromatography, stirred tank adsorption, moving bed chromatography, simulated moving bed chromatography, Fluidized Bed Chromatography and/or Expanded Bed Chromatography.
  • the particulate material may preferably be used as a adsorbent in Fluidized Bed Chromatography and/or Expanded Bed Chromatography.
  • a preferred embodiment of the present invention relates to a method of producing a particulate material, said method comprises the steps of: (i) Suspend a non-porous material and a porous polymeric material in water providing a porous polymeric material suspension;
  • step (ii) Heating the porous polymeric material suspension of step (i) to a
  • the non-porous material comprises a titanium dioxide (T1O2).
  • the heating temperature in step (ii) is above 85°C, such as above 90°C, e.g. in the range of 80-110°C, such as in the range of 90-100°C, e.g. in the range of 92-95°C.
  • the temperature in step (iv) may preferably be reduced to a temperature in the range of 45-70°C, such as in the range of 50-65°C, such as about 60°C.
  • the particle size of the particulate material may be determined by the energy input from the agitation.
  • the agitation provided in step (iv) may be provided by an inline mixer.
  • the inline mixer may be providing an energy input of 1000-10.000 rpm (rounds per minute), such as 2000-8000 rpm, e.g. 3000-5000 rpm, such as about 4000 rpm.
  • a cooling mixture may be added to the porous polymeric material suspension just before the porous polymeric material suspension is subjected to the agitation in step (iv).
  • the term "just before” relates to the process of adding the cooling mixture as close to porous polymeric material suspension is getting in contact with a vortex part of the inside mixer.
  • the cooling mixture may have a temperature in the range of -5-15°C, such as in the range of 0-10°C, e.g. in the range of 2-8°C.
  • the cooling mixture comprises a Vaseline oil.
  • the method of the present invention may further comprise the step of washing.
  • the particulate material obtained in step (v) may be washed with a washing solution.
  • the washing solution may have a temperature in the range of 30-70°C, such as in the range of 40-60°C
  • the washing solution comprises SDS.
  • the method according to the present invention may further comprise the step of sieving the particulate material in order to provide particular particle size fractions.
  • the method comprises the step of sieving the particle material obtained in step (v).
  • the particulate material obtained in step (v) is size separated, preferably using a nylon mesh.
  • 35 g agarose D3 and 40 g T1O2 (grain size ⁇ 21 nm; MW: 79.87; density; 4.26 g/ml) are suspended in 1 L H2O and the mixture is heated to 92-95°C. If desired tungsten carbide may be added to the suspension. The mixture is placed in a preheated water bath at 60°C, ensure that cold air does not cool the solution below 40°C.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Polymers & Plastics (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention relates to a particulate material comprising a particle comprising a non-porous material surrounded by a porous polymeric material, wherein the non-porous material comprises a titanium dioxide (TiO2).

Description

ADSORBENT COMPRISING METAL DIOXIDE AND A POLYMERIC MATERIAL
Technical field of the invention
The present invention relates to a novel particulate material . In particular, the present invention relates to a novel particulate material comprising titanium dioxide for use as an adsorbent in downstream processing of liquid mixtures.
Background of the invention
particulate materials have been used for years in processes of purifying compounds from complex medias like fermentation broths, plant extracts, and body fluids like blood and milk. There is a continuing need a demand from the industry to provide new particulate materials as the presently provided particulate materials may different disadvantages like leaking of particulate material, stability, functionality, addition of several undesirable components either coupled on the particulate material or used during the production of the particulate material .
Hence, an improved particulate material would be advantageous, and in particular, a particulate material that meets some of the above mentioned issues with the particulate material presently provided would be advantageous. Summary of the invention
Thus, an object of the present invention relates to a new particulate material .
In particular, it is an object of the present invention to provide a particulate material and a method that solves the above mentioned problems of the prior art.
Thus, one aspect of the invention relates to a particulate material comprising a particle comprising a non-porous material surrounded by a porous polymeric material, wherein the non-porous material comprises a titanium dioxide (TiCh) . Another aspect of the present invention relates to a method of producing a particulate material, said method comprises the steps of:
(i) Suspend a non-porous material and a porous polymeric material in water providing a porous polymeric material suspension;
(ii) Heating the porous polymeric material suspension of step (i) to a
temperature above 80°C;
(iii) Optionally add a further non-porous material to the porous polymeric
material suspension;
(iv) Reduce the temperature to a temperature between 40-75°C and subject the porous polymeric material suspension to agitation;
(v) Continue the agitation while cooling the porous polymeric material
suspension providing the particulate material; and
(vi) Optionally washing the particulate material obtained; wherein the non-porous material comprises a titanium dioxide (T1O2).
Yet another aspect of the present invention relates to the use of the particulate material according to anyone of claims 1-18 as an adsorbent for isolating one or more compounds from a liquid mixture.
The present invention will now be described in more detail in the following.
Detailed description of the invention
As mentioned above there is a need in the industry for a new particulate material for isolating compounds from complex medias like fermentation broths, plant extracts, and body fluids like blood and milk. The particulate material according to the present invention may preferably be suitable for isolating compounds from fermentation broths, plant extracts, and milk. In an embodiment of the present invention, the liquid mixture may be a primary dairy source.
In the present context, the term "primary dairy source" relates to a diary source comprising one or more milk oligosaccharides.
The primary diary source may preferably comprise one or more milk oligosaccharides and casein.
In an embodiment of the present invention the dairy source may be selected from the group consisting of milk, whole milk, skimmed milk, milk concentrates, reconstituted milk powder, non-pasteurised milk, micro-filtrated milk, pH-adjusted milk, pre-treated dairy source, whey or a fraction obtained from whey.
A characteristic feature of the preliminary dairy source may be that the preliminary dairy source has not been subjected to casein precipitation, removal of casein micelles, and/or removal of the casein aggregates, prior to the separation of one or more oligosaccharide compound(s).
The preliminary dairy source may be obtained as the flow through obtained from a process of separating one or more milk proteins, such as the isolation process of isolation of soluble proteins from aggregated casein-containing mixtures, as described in WO
2016/055064, which is hereby incorporated by reference.
In a preferred embodiment of the present invention related to a particulate material comprising a particle comprising a non-porous material surrounded by a porous polymeric material, wherein the non-porous material comprises a titanium dioxide (T1O2).
In the present context, the term "non-porous material" relates to a material that does not allow a liquid mixture to diffuse inside the material.
In the present context, the term "porous polymeric material" relates to a material that allows a liquid mixture to diffuse inside the material.
The titanium dioxide present in the particulate material may have different forms and structures. Preferably, the particulate material comprises multiple titanium dioxide grains. In an embodiment of the present invention the titanium dioxide grain may have a mean grain size in the range of 10-100 nm, such as in the range of 12-75 nm, e.g. in the range of 15-50 nm, such as in the range of 18-30 nm, e.g. about 21 nm.
The multiple titanium dioxide grains, or the multiple non-porous grains, may be held together by the porous polymeric material.
Preferably the porous polymeric material may be an organic porous polymeric material. In an embodiment of the present invention the porous polymeric material or the organic porous polymeric material may be selected from agarose, alginate, chitosan, carrageenan, and/or pectin. Preferably, the organic porous polymeric material is agarose.
In order to further control the density of the particulate material, the particulate material may comprise a further non-porous material. Hence, in an embodiment of the present invention the particulate material may comprise a further non-porous material in addition to the titanium dioxide.
In the present context, the term "further non-porous material" relates to a non-porous material different from titanium dioxide which may be included into the particulate material, resulting in a particulate material having at least two different types of non- porous materials.
In an embodiment of the present invention wherein the further non-porous material may be selected from a high density non-porous material; a silicate; a ceramic metal; alumina; or a magnetic material. Further examples of non-porous materials, (non-porous core materials) are described in WO 2010/037736, which is hereby incorporated by reference.
In another embodiment of the present invention the high density non-porous material has a density of at least 4.0 g/ml, such as at least 10 g/ml, e.g. at least 16 g/ml, such as at least 25 g/ml. Typically, the non-porous core material has a density in the range of about 4.0-25 g/ml, such as about 4.0-20 g/ml, e.g. about 4.0-16 g/ml, such as 12-19 g/ml, e.g. 14-18 g/ml, such as about 6.0-15.0 g/ml, e.g. about 6.0-16 g/ml.
Preferably, the high density non-porous material may be tungsten carbide or steel or a combination hereof.
The non-porous material may constitute at least 10% (w/w), of the particulate material, such as at least 20% (w/w), e.g. at least 30%, such as at least 40% (w/w), e.g. at least 50%, such as at least 55% (w/w), e.g. at least 60%, such as at least 65% (w/w), e.g. at least 70%.
The content of titanium dioxide may preferably constitute at least 10% (w/w), of the particulate material, such as at least 20% (w/w), e.g. at least 30%, such as at least 40% (w/w), e.g. at least 50%, such as at least 55% (w/w), e.g. at least 60%, such as at least 65% (w/w), e.g. at least 70%.
The porous polymeric material may constitute at least 30% (w/w), of the particulate material, such as at least 40% (w/w), e.g. at least 50%, such as at least 55% (w/w), e.g. at least 60%, such as at least 65% (w/w), e.g. at least 70%, such as at least 80% (w/w), e.g. at least 90%.
The density of the adsorbent according to the present invention relates to the density of an adsorbent in it's fully solvated (e.g. hydrated) state as opposed to the density of a dried adsorbent particle.
The desired density of the one or more adsorbent may be provided by inclusion of a certain proportion or a certain amount of the non-porous material in the porous polymeric material.
In an embodiment of the present invention the particulate material may have a density of at least 1.1 g/ml, more preferably at least 1.3 g/ml, still more preferably at least 1.5 g/ml, even more preferably at least 1.8 g/ml, even more preferably at least 2.0 g/ml, even more preferably at least 2.3 g/ml, even more preferably at least 2.5 g/ml, even more preferably at least 2.75 g/ml, even more preferably at least 3.0 g/ml, even more preferably at least 3.5 g/ml, even more preferably at least 4.0 g/ml.
Preferably at least 95% of the particulate material is substantially spherical.
In a preferred embodiment of the present invention the particulate material may be an adsorbent or part of an adsorbent material.
Traditionally a ligand is coupled to the particulate material when using the particulate material as an adsorbent, e.g. in isolating compounds from complex medias like fermentation broths, plant extracts, and body fluids like blood and milk, however, titanium dioxide as used as non-porous material according to the present invention, may preferably as a ligand for isolating compounds from complex medias, or liquid media. In an embodiment of the present invention, the one or more compounds to be isolated from the liquid mixture may preferably be one or more oligosaccharide compound.
In a further embodiment of the present invention the one or more oligosaccharide compound(s) comprises at least one moiety selected from the group consisting of a sialic acid moiety; Hexose moiety (a Hex moiety); a HexNAc moiety; and a NeuAc moiety.
Preferably the one or more oligosaccharide compound(s) comprises at least one moiety selected from a sialic acid moiety or a NeuAc moiety as the terminal moiety of the oligosaccharide. In an embodiment of the present invention the adsorbent comprising a ligand. Preferably, the non-porous material of the adsorbent, the titanium dioxide, is acting as the ligand.
The particulate material according to the present invention may preferably be used as a chromatographic support. The chromatographic support may be a membrane
chromatography support, or a column chromatography support. Preferably, the column chromatography support includes a Packed Bed Chromatography, stirred tank adsorption, moving bed chromatography, simulated moving bed chromatography, Fluidized Bed Chromatography and/or Expanded Bed Chromatography. The particulate material may preferably be used as a adsorbent in Fluidized Bed Chromatography and/or Expanded Bed Chromatography.
A preferred embodiment of the present invention relates to a method of producing a particulate material, said method comprises the steps of: (i) Suspend a non-porous material and a porous polymeric material in water providing a porous polymeric material suspension;
(ii) Heating the porous polymeric material suspension of step (i) to a
temperature above 80°C;
(iii) Optionally add a further non-porous material to the porous polymeric
material suspension;
(iv) Reduce the temperature to a temperature between 40-75°C and subject the porous polymeric material suspension to agitation;
(v) Continue the agitation while cooling the porous polymeric material
suspension providing the particulate material; and (vi) Optionally washing the particulate material obtained; wherein the non-porous material comprises a titanium dioxide (T1O2).
Preferably, the heating temperature in step (ii) is above 85°C, such as above 90°C, e.g. in the range of 80-110°C, such as in the range of 90-100°C, e.g. in the range of 92-95°C.
The temperature in step (iv) may preferably be reduced to a temperature in the range of 45-70°C, such as in the range of 50-65°C, such as about 60°C.
The particle size of the particulate material may be determined by the energy input from the agitation.
In an embodiment of the present invention the agitation provided in step (iv) may be provided by an inline mixer. Preferably, the inline mixer may be providing an energy input of 1000-10.000 rpm (rounds per minute), such as 2000-8000 rpm, e.g. 3000-5000 rpm, such as about 4000 rpm.
In an embodiment of the present invention a cooling mixture may be added to the porous polymeric material suspension just before the porous polymeric material suspension is subjected to the agitation in step (iv).
In the present context, the term "just before" relates to the process of adding the cooling mixture as close to porous polymeric material suspension is getting in contact with a vortex part of the inside mixer.
In an embodiment of the present invention the cooling mixture may have a temperature in the range of -5-15°C, such as in the range of 0-10°C, e.g. in the range of 2-8°C.
Preferably, the cooling mixture comprises a Vaseline oil.
The method of the present invention may further comprise the step of washing. Hence, preferably, the particulate material obtained in step (v) may be washed with a washing solution.
The washing solution may have a temperature in the range of 30-70°C, such as in the range of 40-60°C
In an embodiment of the present invention the washing solution comprises SDS. The method according to the present invention may further comprise the step of sieving the particulate material in order to provide particular particle size fractions. In an embodiment of the present invention the method comprises the step of sieving the particle material obtained in step (v).
Preferably, the particulate material obtained in step (v) is size separated, preferably using a nylon mesh.
It should be noted that embodiments and features described in the context of one of the aspects of the present invention also apply to the other aspects of the invention.
All patent and non-patent references cited in the present application, are hereby incorporated by reference in their entirety.
The invention will now be described in further details in the following non-limiting examples.
Examples
Production of agarose beads containing Ti02.
In a 2 L beaker 35 g agarose D3 and 40 g T1O2 (grain size~21 nm; MW: 79.87; density; 4.26 g/ml) are suspended in 1 L H2O and the mixture is heated to 92-95°C. If desired tungsten carbide may be added to the suspension. The mixture is placed in a preheated water bath at 60°C, ensure that cold air does not cool the solution below 40°C.
Simultaneously pumping the warm agarose suspension and 2-8°C Vaseline oil into an inline mixer set to 4000 rpm. The two flows must be pumped together just before they enter the vortex inside the inline mixer. The flows must be adjusted to ensure that the temperature of the flow coming out of the inline mixer is below 30°C. The oil suspended agarose beads formed are collected, and wash them multiple times with 0.1% SDS at 40-60°C. The particles can be size separated on nylon mesh if desired or utilized as is. References
WO 2010/037736

Claims

Claims
1. A particulate material comprising a particle comprising a non-porous material surrounded by a porous polymeric material, wherein the non-porous material comprises a titanium dioxide (T1O2) .
2. The particulate material according to claim 1, wherein the particulate material comprises multiple titanium dioxide grains.
3. The particulate material according to claim 2, wherein the titanium dioxide grain has a mean grain size in the range of 10-100 nm, such as in the range of 12-75 nm, e.g . in the range of 15-50 nm, such as in the range of 18-30 nm, e.g . about 21 nm.
4. The particulate material according to anyone of the preceding claims, wherein the porous polymeric material is an organic porous polymeric material, the organic porous polymeric material may be selected from agarose, alginate, chitosan, carrageenan, and/or pectin.
5. The particulate material according to anyone of the preceding claims, wherein the particulate material comprises a further non-porous material in addition to the titanium dioxide.
6. The particulate material according to claim 5, wherein the further non-porous material is selected from a high density non-porous material; a silicate; a ceramic metal; alumina; or a magnetic material .
7. The particulate material according to claim 6, wherein the high density non-porous material has a density of at least 4.0 g/ml, such as at least 10 g/ml, e.g . at least 16 g/ml, such as at least 25 g/ml. Typically, the non-porous core material has a density in the range of about 4.0-25 g/ml, such as about 4.0-20 g/ml, e.g. about 4.0-16 g/ml, such as 12-19 g/ml, e.g. 14-18 g/ml, such as about 6.0-15.0 g/ml, e.g . about 6.0-16 g/ml .
8. Use of the particulate material according to anyone of claims 1-7 as an adsorbent for isolating one or more compounds from a liquid mixture.
9. The use according to claim 8, wherein the one or more compounds is one or more oligosaccharide compound .
10. The use according to anyone of claims 8 or 9, wherein the liquid mixture is a primary dairy source.
PCT/EP2018/084969 2017-12-17 2018-12-14 Adsorbent comprising metal dioxide and a polymeric material WO2019115772A1 (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020104801A1 (en) * 1998-04-06 2002-08-08 Nicolas Voute Small dense microporous solid support materials, their preparation,and use for purification of large macromolecules and bioparticles
US20050065329A1 (en) * 2001-06-01 2005-03-24 Upfront Chromatography A/S Fractionation of protein containing mixtures
US20060177855A1 (en) * 2005-01-21 2006-08-10 Utermohlen Joseph G Nanoparticles for manipulation of biopolymers and methods of thereof
US20070092960A1 (en) * 2003-03-21 2007-04-26 Upfront Chromatography A/S Method for high throughput volumes in the fractionation of bio-molecules by chromatographic systems
WO2010037736A1 (en) * 2008-09-30 2010-04-08 Upfront Chromatography A/S A METHOD FOR PROVIDING A β-LACTOGLOBULIN PRODUCT AND AN α-ENRICHED WHEY PROTEIN ISOLATE
US20100294977A1 (en) * 2008-02-15 2010-11-25 Ge Healthcare Bio-Sciences Ab Separation of biomolecules

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020104801A1 (en) * 1998-04-06 2002-08-08 Nicolas Voute Small dense microporous solid support materials, their preparation,and use for purification of large macromolecules and bioparticles
US20050065329A1 (en) * 2001-06-01 2005-03-24 Upfront Chromatography A/S Fractionation of protein containing mixtures
US20070092960A1 (en) * 2003-03-21 2007-04-26 Upfront Chromatography A/S Method for high throughput volumes in the fractionation of bio-molecules by chromatographic systems
US20060177855A1 (en) * 2005-01-21 2006-08-10 Utermohlen Joseph G Nanoparticles for manipulation of biopolymers and methods of thereof
US20100294977A1 (en) * 2008-02-15 2010-11-25 Ge Healthcare Bio-Sciences Ab Separation of biomolecules
WO2010037736A1 (en) * 2008-09-30 2010-04-08 Upfront Chromatography A/S A METHOD FOR PROVIDING A β-LACTOGLOBULIN PRODUCT AND AN α-ENRICHED WHEY PROTEIN ISOLATE

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