EP0183207A1 — Porous glass fibers with immobilized biochemicall…

Claim 1

Independent Claim 105 words

Porous glass material with immobilized biochemically active material, characterized in that: a. the porous glass material is in the form of at least one porous silica-rich fiberous material having dimensions varying from fiberous particles to fibers having a diameter of around 3 microns to around 150 microns and a length of around 0.03 inch to continuous fiber length and having pores with a mean pore diameter in the range of about 10 angstroms to about 3000 angstroms, and b. biochemically active material is surrounded by an activity maintaining environment where the biochemically active material are present on at least one surface of the fiberous material.

Claim 2

Dependent Claim 105 words

Porous glass material with immobilized biochemically active material, characterized in that: a. the porous glass material is in the form of at least one porous silica-rich fiberous material having dimensions varying from fiberous particles to fibers having a diameter of around 3 microns to around 150 microns and a length of around 0.03 inch to continuous fiber length and having pores with a mean pore diameter in the range of about 10 angstroms to about 3000 angstroms, and b. biochemically active material is surrounded by an activity maintaining environment where the biochemically active material are present on at least one surface of the fiberous material.

Claim 3

Dependent Claim 97 words

Porous glass material of Claim 1 formed from the alkali metal oxide borosilicate ternary glass composition system, wherein B 2 0 3 is present in an amount of greater than 35 weight percent up to around 60 weight percent, SiO 2 in an amount in the range of 30 to about 65 weight percent, alkali metal oxide present in an amount of about 5 to about 15 weight percent, zirconium oxide present in an amount of about 0 to about 5 weight percent and aluminum oxide present in an amount of about 0 to 4 weight percent.

Claim 4

Dependent Claim 21 words

Porous glass material of Claims 1 or 2, having a fiber diameter from around 3 microns to less than 40 microns.

Claim 5

Dependent Claim 26 words

Porous glass material of Claims 1-3 that are hollow porous, silica rich glass fibers having a K factor in the range of up to about 0.9.

Claim 6

Dependent Claim 51 words

Porous glass material of Claims 1-4, wherein between the biochemically active material and the internal and external surfaces of the porous fiberous material there is present one or more chemical attaching agents in a sufficient amount to constitute a monolayer over a substantial portion of the surfaces of the fiberous material.

Claim 7

Dependent Claim 22 words

Porous glass material of Claims 1-5 having a surface area of about 10 m 2 /gm to about 600 m 2 /gm.

Claim 8

Dependent Claim 27 words

Porous glass material of Claim 5, wherein the attaching agent is selected from the group consisting of gamma aminopropyltriethoxy silane, silyl aldehyde organo silanes or mixtures thereof.

Claim 9

Dependent Claim 40 words

Porous glass material of Claims 5 or 7, wherein in addition to the attaching agent there is present an intermediate compound reactable with the organic functional end of the organo silane and an organic moiety on the biochemically active material.

Claim 10

Independent Claim 245 words

A method of producing porous glass material having immobilized biochemically active material, characterized in that: a. forming the glass material into fibers from fiberizable, pore generating, glass forming batch composition formulated to result in a glass composition having an amount of leachable materials that yield pores upon leaching where the pores have a mean pore diameter at least greater than the minimum exclusion diameter of nonliving biochemically active material and greater than the minimum exclusion diameter of related materials for living biochemically active materials, b. attenuating the glass fibers, c. generating pores in the glass fibers by removing leachable components selected from the group consisting of water leachable, acid leachable and alkali leachable materials and water and acid leachable materials, water and acid and alkali leachable materials, and acid and alkali leachable materials to produce porous fiberous material with substantial amounts of silica and with dimensions varying from particles to continuous lengths of fibers, where the mean pore diameter of the pores is at least greater than the minimum exclusion diameter of the nonliving biochemically active material and at least greater than the minimum exclusion diameter of related materials for living biochemically active material and where the pore volume is sufficient to provide a larger internal surface area than external surface area for the fiberous materials, d. contacting the porous fiberous materials with one or more biochemically active materials to immobilize them in the internal surface and on the external surface of the fiberous materials.

Claim 11

Independent Claim 245 words

A method of producing porous glass material having immobilized biochemically active material, characterized in that: a. forming the glass material into fibers from fiberizable, pore generating, glass forming batch composition formulated to result in a glass composition having an amount of leachable materials that yield pores upon leaching where the pores have a mean pore diameter at least greater than the minimum exclusion diameter of nonliving biochemically active material and greater than the minimum exclusion diameter of related materials for living biochemically active materials, b. attenuating the glass fibers, c. generating pores in the glass fibers by removing leachable components selected from the group consisting of water leachable, acid leachable and alkali leachable materials and water and acid leachable materials, water and acid and alkali leachable materials, and acid and alkali leachable materials to produce porous fiberous material with substantial amounts of silica and with dimensions varying from particles to continuous lengths of fibers, where the mean pore diameter of the pores is at least greater than the minimum exclusion diameter of the nonliving biochemically active material and at least greater than the minimum exclusion diameter of related materials for living biochemically active material and where the pore volume is sufficient to provide a larger internal surface area than external surface area for the fiberous materials, d. contacting the porous fiberous materials with one or more biochemically active materials to immobilize them in the internal surface and on the external surface of the fiberous materials.

Claim 12

Dependent Claim 22 words

Method of Claim 9, which includes maintaining the activity of the biochemically active material immobilized on and in the glass fiberous materials.

Claim 13

Dependent Claim 23 words

Method of Claims 9 or 10, which includes gathering the fibers into at least one strand before generating pores in the glass fibers.

Claim 14

Dependent Claim 21 words

Method of Claims 9-11, which includes treating the filaments with an aqueous chemical treating composition before gathering the filaments into strands.

Claim 15

Dependent Claim 26 words

Method of Claim 12, which includes removing any residue of the aqueous chemical treating composition before contacting the porous silica-rich fibers with the biochemically active material.

Claim 16

Dependent Claim 27 words

Method of Claims 9-13, wherein the fibers are attenuated mechanically and gathered into at least one strand and wound on a winder in a multilayered cylindrical package.

Claim 17

Dependent Claim 64 words

Method according to Claims 9-14, wherein at least one strand is removed from the multilayered package and cut to have a length from about 1 to about 64 inches which includes maintaining the alignment of the discrete lengths of fibers in near parallel alignment during pore generation, contacting the fibers with a biochemically active material and maintaining the activity of the biochemically active material.

Claim 18

Dependent Claim 92 words

Method of Claims 9-15, wherein the glass fibers are formed to have a silica-poor group of at least about 15 volume percent of the glass composition having leachable materials selected from water leachable inorganic oxides, acid leachable inorganic oxides and a mixture thereof and a silica-rich group selected from silica and silica and inorganic oxide glass modifiers, wherein the amount of silica is less than around 85 volume percent of the glass composition and, wherein the fibers are heat treated to phase separate the two groups before leaching to generate the pores.

Claim 19

Dependent Claim 30 words

Method of Claim 16, wherein the amount of the silica-poor group is greater than around 35 weight percent of the glass fibers and the heat treated fibers are water leached.

Claim 20

Dependent Claim 13 words

Method of Claims 16-17, wherein the water leached glass fibers are acid leached.

Claim 21

Dependent Claim 46 words

Method of Claims 16-18, wherein the silica-poor group is comprised of boron-containing material and alkali metal oxides from an alkali metal borosilicate glass fiber composition and the amount of boron oxide is greater than 35 weight percent up to 60 weight percent of the glass composition.

Claim 22

Dependent Claim 25 words

Method of Claims 16-19, wherein the amount of silica in the glass composition is greater than around 25 weight percent of the glass fiber composition.

Claim 23

Dependent Claim 35 words

Method of Claims 16-20, wherein the silica-poor group of inorganic oxides are removed by nonalkaline leaching and the porous fibers are alkali leached to give a pore volume of about 0.5 to about 1.2 cc/gm.

Claim 24

Dependent Claim 89 words

Method of Claims 16-21, wherein the fibers are heat treated at a temperature in the range of about 400 to about 600°C for a period of time in the range of about 10 minutes to about 64 hours to phase separate the glass fibers, and cooling the phase separated fibers to avoid thermal cracking, water leaching the glass fibers at an elevated temperature, acid leaching the fibers at an elevated temperature to remove the water and acid leachable components of the fibers to produce the porous silica-rich glass fibers.

Claim 25

Dependent Claim 49 words

Method of Claims 9-15, wherein fiberous particulates are produced from glass fibers having less than around 30 weight percent silica and a remainder of inorganic oxides selected from the group consisting of water leachable, inorganic oxides, acid leachable inorganic oxides, and mixtures thereof by removing the leachable inorganic oxides.

Claim 26

Dependent Claim 16 words

Method of Claim 23, wherein the leachable inorganic oxides are removed by heat treating and leaching.

Claim 27

Dependent Claim 28 words

Method of Claims 9-15, wherein the glass fiber particulates are produced from glass fibers by alkali leaching to yield a pore volume of greater than around 1.2 cc/gm.

Claim 28

Dependent Claim 98 words

Method of Claims 9-22, wherein the glass fibers have a first silica-poor group of inorganic oxides selected from the group consisting of water leachable inorganic oxides, acid leachable inorganic oxides and mixtures thereof and a second silica-rich group of non-water and essentially non-acid leachable inorganic oxides having less than around 85 weight percent of the glass composition as silica, wherein inorganic oxides in the first group are leached and the leached fibers are alkali leached to remove silica to give a pore volume in the porous glass fibers in the range of about 0.5 to about 1.5 cc/gm.

Claim 29

Dependent Claim 18 words

Method of Claim 30, wherein the glass fibers have a fiber diameter of less than around 20 microns.

Claim 30

Dependent Claim 42 words

Method of Claims 9-27, wherein at least one linking agent is applied to the porous fibers before contacting with the biochemically active material in a sufficient amount to provide linking agent for the internal and external surface area of the porous fibers.

Claim 31

Dependent Claim 31 words

Method of Claim 28, wherein the amount of linking agent is that sufficient to provide a monolayer of linking agent for the internal and external surface areas of the porous fibers.

Claim 32

Dependent Claim 16 words

Method of Claims 28-29, wherein the linking agent is used in conjunction with an intermediate compound.

Claim 33

Dependent Claim 18 words

Method of Claims 28-30, wherein the linking agent is gamma aminopropyltriethoxy silane and the intermediate compound is glutaraldehyde.

Claim 34

Dependent Claim 24 words

Method of Claims 28-30, wherein the linking agent is selected from the group consisting of a silyl aldehyde organo silane and gamma aminopropyltriethoxy silane.

Claim 35

Dependent Claim 35 words

Method of Claims 28-30, wherein the linking agent is an organo silane coupling agent to place a positive charge on the fiber which is reacted with collagen and affiliated with lysine for attaching cellular biomaterial.

Claim 36

Dependent Claim 15 words

Method of Claims 9-33, wherein the biochemically active material is one or more enzymes. -

Claim 37

Dependent Claim 29 words

Method of Claims 9-33, wherein the biochemically active material is one or more cells, wherein the cells are immobilized only on the external surface area of the porous fibers.

Claim 38

Dependent Claim 18 words

Method of Claims 28-35, which includes removing any entrapped air from the porous fiber having the linking agent.

Claim 39

Dependent Claim 25 words

Glass fibers produced by the method of Claims 9-36, wherein the fibers have diameters ranging from around less than 3 microns to about 150 microns.

Claim 40

Dependent Claim 22 words

Glass fibers produced by the method of Claims 9-36, wherein the fibers have diameters of up to less than around 40 microns.

Claim 41

Dependent Claim 15 words

Glass fibers produced according to the method of Claims 9-36, which are hollow glass fibers.

Claim 42

Dependent Claim 23 words

Glass fibers produced according to the method of Claims 9-36, having a discrete legnth of less than(l inch) .2.54 cm to continuous fibers.

Porous glass fibers with immobilized biochemically active material

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