EP0050864A1
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EP
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A hydrophilic cationic charge modified microporous membrane, a process for producing it and its use
Assignee: 3M Purification Inc
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Filing: 1981-10-23
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Granted: —
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Expires: 2001-10-23
Abstract
Abstract A novel cationic charge modified microporous membrane is provided comprising a hydrophilic organic polymeric microporous membrane and a charge modifying amount of a primary cationic charge modifying agent bonded to substantially all of the wetted surfaces of the membrane. The primary charge modifying agent is a water soluble organic polymer having a molecular weight greater than about 1000 wherein each monomer thereof has at least one epoxide group capable of bonding to the surface of the membrane and at least one tertiary amine or quaternary ammonium group Preferably, a portion of the epoxy groups on the organic polymer are bonded to a secondary charge modifying agent selected from the group consisting of: i) aliphatic amines having at least one primary amine or at least two secondary amines; and ii) aliphatic amines having at least one secondary amine and a carboxyl or hydroxyl substituent. The invention is further directed to a process for cationically charge modifying a hydrophilic organic polymeric microporous membrane by applying to the membrane the aforesaid charge modifying agents, preferably, by contacting the membrane with aqueous solutions of the charge modifying agents. The preferred microporous membrane is nylon, the preferred primary and secondary charge modifying agents are, respectively, polyamido-polyamine epichlorohydrin and tetraethylene pentamine. The invention is further directed to a process for improving the responsiveness of a nylon membrane to charge modification, comprising chemically treating the membrane to provide enhanced ninhydrin response evidencing free amino functionality. The charge modified microporous membrane of this invention may be used for the filtration of fluids, particularly parenteral or biological liquids. The membrane has low extractables and is sanitizable or sterilizable.
Inventors
- 👤 Eugene A. Ostreicher
- 👤 Rodney A. Knight
- 👤 Joseph V. Fiore
- 👤 George T. Emond
- 👤 Kenneth C. Hou
Bibliographic Details
Application Number
—
Jurisdiction
EP
Data Source
google_patents
Last Synchronized
2026-10-31 16:01
CPC Classifications
B; B01; B01D; B01D67/00; B01D67/0081; B01D67/0093; A; A61; A61K; A61K35/00; A61K35/12; A61K35/14; A61K35/16; A61L; A61L2/00; A61L2/02; A61L2/022; B01D67/0002; B01D67/0009; B01D67/0011; B01D67/00111; B01D71/00; B01D71/06; B01D71/56; A61L2103/00; A61L2103/05; A61L2103/09; A61L2103/10; B01D2323/00; B01D2323/08; B01D2323/30; B01D2325/00; B01D2325/14; B01D2325/36
Claims Analysis
Total Claims: 59
Claim 1
Independent Claim
78 words
A cationic charge modified microporous membrane comprising a hydrophilic organic polymeric microporous membrane and a charge modifying agent bonded to substantially all of the wetted surfaces of the membrane, the primary charge modifying agent being a water soluble organic polymer having a molecular weight greater than about 1000, wherein each monomer thereof has at least one epoxide group capable of bonding to the surface of the membrane and at least one tertiary a mine or quaternary ammonium group.
Claim 2
Dependent Claim
78 words
A cationic charge modified microporous membrane comprising a hydrophilic organic polymeric microporous membrane and a charge modifying agent bonded to substantially all of the wetted surfaces of the membrane, the primary charge modifying agent being a water soluble organic polymer having a molecular weight greater than about 1000, wherein each monomer thereof has at least one epoxide group capable of bonding to the surface of the membrane and at least one tertiary a mine or quaternary ammonium group.
Claim 3
Dependent Claim
62 words
The nicroporous membrane of claim 1, wherein a portion of the epoxy groups on the organic polymer are bonded to a secondary charge modifying agent selected from the group consisting of: i) aliphatic amines having at least one primary amine or at least two secondary amines; and ii) aliphatic amines having at least one secondary amine and a carboxyl or hydroxyl substituent..
Claim 4
Dependent Claim
18 words
The microporous membrane of claim 1 or 2, wherein the hydrophilic organic polymeric microporous membrane is polyvinylidene fluoride.
Claim 5
Dependent Claim
19 words
The microporous membrane of claim 1 or 2, wherein the hydrophilic organic polymeric microporous membrane is esters of cellulose.
Claim 6
Dependent Claim
17 words
The microporous membrane of claim 1 or 2, wherein the hydrophilic organic polymeric microporous membrane is nylon.
Claim 7
Dependent Claim
18 words
The microporous membrane of claim 1 or 2, wherein the hydrophilic organic polymeric microporous membrane is polyhexamethylene adipamide.
Claim 8
Dependent Claim
17 words
The microporous membrane of claim 1 or 2, wherein the charged modified membrane is sanitized or sterilized.
Claim 9
Dependent Claim
19 words
The microporous membrane of claim 1 or 2, wherein the primary charge modifying agent is a polyamido-polyamine epichlorohydrin resin.
Claim 10
Dependent Claim
41 words
The microporous membrane of claim 2, wherein the secondary charge modifying agent is an amine of the formula: wherein R 1 and R 2 are alkyl of 1 to 4 carbon atoms and x is an integer from 0 to 4.
Claim 11
Dependent Claim
17 words
The microporous membrane of claim 9 wherein the primary charge modifying agent is a polyamido-polyamine epichlorohydrin resin.
Claim 12
Dependent Claim
18 words
The microporous membrane of claim 9 or 10, wherein the a mine is tetraethylene pentamine of the formula:
Claim 13
Dependent Claim
12 words
The microporous membrane of claim 11, wherein the nylon is polyhexamethylene adipamide.
Claim 14
Dependent Claim
133 words
The microporous membrane of claim 5 wherein the microporous membrane is prepared by a process co m prising: (a) preparing a dope solution of a nylon polymer in a solvent system comprising a mixture of at least one solvent and one non-solvent for the polymer, the amount of non-solvent being no greater than an amount required to induce nucleation of the solution to obtain a visible precipitate, said solvent being formic acid and said non- solvent being selected from the group consisting of methanol, methyl formate, water and glycerol; (b) directly casting said solution under the surface of a quenching bath comprising a non-solvent system for said polymer for a time sufficient to form micropores in said film, said non-solvent system being a mixture of methanol and water or formic acid and water.
Claim 15
Dependent Claim
86 words
A process for cationically modifying a hydrophilic organic polymeric microporous membrane comprising applying to the membrane a charge modifying amount of a primary cationic charge modifying agent bonded to substantially all of the wetted surface of the membrane, the primary charge modifying agent being a water soluble organic polymer having a molecular weight greater than about 1000, wherein each monomer thereof has at least one epoxide group capable of bonding to the surface of the membrane and at least one tertiary amine or quaternary ammonium group.
Claim 16
Dependent Claim
86 words
A process for cationically modifying a hydrophilic organic polymeric microporous membrane comprising applying to the membrane a charge modifying amount of a primary cationic charge modifying agent bonded to substantially all of the wetted surface of the membrane, the primary charge modifying agent being a water soluble organic polymer having a molecular weight greater than about 1000, wherein each monomer thereof has at least one epoxide group capable of bonding to the surface of the membrane and at least one tertiary amine or quaternary ammonium group.
Claim 17
Dependent Claim
62 words
The process of claim 14, wherein a portion of the epoxy groups on the organic polymer are bonded to a secondary charge modifying agent selected from the group consisting of: i) aliphatic amines having at least one prim ary amine or at least two secondary amines; and ii) aliphatic amines having at least one secondary amine and a carboxyl or hydroxyl substituent.
Claim 18
Dependent Claim
133 words
A process for cationically modifying a hydrophilic organic polymeric microporous membrane comprising: a) contacting the membrane with an aqueous solution of a primary cationic charge modifying agent, the primary charge modifying agent being a water soluble organic polymer having a molecular weight greater than 1000 wherein each monomer thereof has at least one epoxide group capable of bonding to the surface of the membrane and at least one tertiary amine or quaternary ammonium group; b) contacting the membrane with an aqueous solution of a secondary cationic charge modifying agent, the secondary charge modifying agent being selected from the group consisting of: i) aliphatic amines having at least one primary amine or at least two secondary amines; and ii) aliphatic amines having at least one secondary a mine and a carboxyl or hydroxyl substituent.
Claim 19
Dependent Claim
133 words
A process for cationically modifying a hydrophilic organic polymeric microporous membrane comprising: a) contacting the membrane with an aqueous solution of a primary cationic charge modifying agent, the primary charge modifying agent being a water soluble organic polymer having a molecular weight greater than 1000 wherein each monomer thereof has at least one epoxide group capable of bonding to the surface of the membrane and at least one tertiary amine or quaternary ammonium group; b) contacting the membrane with an aqueous solution of a secondary cationic charge modifying agent, the secondary charge modifying agent being selected from the group consisting of: i) aliphatic amines having at least one primary amine or at least two secondary amines; and ii) aliphatic amines having at least one secondary a mine and a carboxyl or hydroxyl substituent.
Claim 20
Dependent Claim
13 words
The process of claim 16, wherein contacting step (a) precedes contacting step (b).
Claim 21
Dependent Claim
19 words
The process of claim 14, 15, 16 or 17, wherein the hyarophilic organic polymeric microporous membrane is polyvinylidene fluoride.
Claim 22
Dependent Claim
20 words
The process of claim 14, 15, 15 or 17, wherein the hydrophilic organic polymeric microporous membrane is esters of cellulose.
Claim 23
Dependent Claim
18 words
The process of claim 14, 15, 16 or 17 wherein the hydrophilic organic polymeric microporous membrane is nylon.
Claim 24
Dependent Claim
18 words
The process of claim 14, 15, 16 or 17, wherein the hydrophilic organic polymeric microporous membrane is polyhexamethylene-adipamide.
Claim 25
Dependent Claim
17 words
The process of claim 14, 15, 16, 17, further comprising subsequently sanitizing or sterilizing the microporous membrane.
Claim 26
Dependent Claim
20 words
The process of claim 14, 15, 16 or 17, wherein the primary charge modifying agent is a polyamido-polyamine epichlorohydrin resin.
Claim 27
Dependent Claim
45 words
The process of claim 15, 16 or 17 wherein the secondary cationic charge modifying agent is an a mine of the formula. wherein R 1 and R 2 are alkyl of 1 to 4 carbon atoms and x is an integer from 0 to 4.
Claim 28
Dependent Claim
17 words
The process of claim 24, wherein the primary charge modifying agent is a polyamido-polya mine epichlorohydrin resin.
Claim 29
Dependent Claim
13 words
The process of claim 24 wherein R 1 and R 2 are ethyl.
Claim 30
Dependent Claim
14 words
The process of claim 25, wherein the amine is tetraethylene pentamine of the formula:
Claim 31
Dependent Claim
13 words
The process of claim 27, wherein the nylon is polyhexa- . methylene adipamide.
Claim 32
Dependent Claim
128 words
The process of claim 20, wherein the membrane is prepared by a process comprising: a) preparing a dope solution of a nylon polymer ina solvent system comprising a mixture of at least one solvent and one non-solvent for the polymer, the amount of non-solvent being no greater than an amount required to induce nucleation of the solution to obtain a visible precipitate, said solvent being formic acid and said non- solvent being selected from the group consisting of methanol, methyl formate, water and glycerol; (b) directly casting said solution under the surface of a quenching bath comprising a non-solvent system for said polymer for a time sufficient to form micropores in said film, said non-solvent system being a mixture of methanol and water or formic acid and water.
Claim 33
Dependent Claim
28 words
The process of claim 16 or 17, wherein the aqueous solution of the primary charge modifying agent contains at least about 1.0% agent by weight of the solution.
Claim 34
Dependent Claim
26 words
The process of claim 33, wherein the aqueous solution of secondary charge modifying agent contains at least about .01 X agent by weight of the solution.
Claim 35
Dependent Claim
27 words
The process of claim 30, wherein the aqueous solution of the primary charge modifying agent contains less than about 5 % agent by weight of the solution.
Claim 36
Dependent Claim
29 words
33 . The process of claim 31, wherein the aqueous solution of the secondary charge modifying agent contains less than about .5 % agent by weight of the solution.
Claim 37
Dependent Claim
29 words
The process of claim 16 or 17, wherein the weight ratio of the primary agent to the secondary agent in the aqueous solutions is from about 2:1 to 500:1.
Claim 38
Dependent Claim
16 words
The process of claim 34, wherein the weight ratio is from about 25:1 to about 75:1.
Claim 39
Dependent Claim
28 words
The process of claim 31, wherein the weight ratio of the primary agent to the secondary agent in the aqueous solutions is from about 2:1 to about 500:1.
Claim 40
Dependent Claim
16 words
The process of claim 36, wherein the weight ratio is from about 25:1 to about 75:1.
Claim 41
Dependent Claim
31 words
The process of claim 20 or 29, further comprising chemically treating the nylon membrane to provide enhanced ninhydrin response evidencing free amino functionality, whereby the responsiveness to charge modification is improved.
Claim 42
Dependent Claim
37 words
The process of claim 38, wherein the chemical treatment is performed prior to applying the primary charge modifying agent to the membrane or prior to contacting the membrane with the aqueous solution of primary charge modifying agent.
Claim 43
Dependent Claim
37 words
The process of claim 38, wherein the chemical treatment is performed simultaneously with applying the primary charge modifying agent to the membrane or simultaneously with contacting the membrane with the aqueous solution of primary charge modifying agent.
Claim 44
Dependent Claim
22 words
The process of claim 39, wherein the membrane is chemically treated with an aqueous solution having a pH greater than about 7.
Claim 45
Dependent Claim
14 words
The process of claim 41, wherein the pH is from about 9 to 11.
Claim 46
Dependent Claim
18 words
The process of claim 42, wherein the aqueous solution is an aqueous solution is comprised of sodium hydroxide.
Claim 47
Dependent Claim
22 words
The process of claim 40, wherein the membrane is chemically treated with an aqueous solution having a pH greater than about 7.
Claim 48
Dependent Claim
14 words
The process of claim 44, wherein the pH.is from about 9 to about 11.
Claim 49
Dependent Claim
17 words
The process of claim 45, wherein the aqueous solution is an aqueous solution comprised of sodium hydroxide.
Claim 50
Dependent Claim
20 words
The process of claim 16 or 17, wherein the aqueous solution is adjusted to a pH greater than about 7.
Claim 51
Dependent Claim
14 words
The process of claim 47, wherein the pH is from about.9 to about 11.
Claim 52
Dependent Claim
16 words
The process of claim 14, 15, 16 or 17 further comprising drying and curing the membrane.
Claim 53
Dependent Claim
24 words
A process for improving the reponsiveness of membrane to charge modification, comprising chemically treating the membrane to provide enhanced minhydrin response evidencingfree amino functionality.
Claim 54
Dependent Claim
24 words
A process for improving the reponsiveness of membrane to charge modification, comprising chemically treating the membrane to provide enhanced minhydrin response evidencingfree amino functionality.
Claim 55
Dependent Claim
22 words
The process of claim 50, wherein the membrane is chemically treated with an aqueous solution having a pH greater than about 7.
Claim 56
Dependent Claim
15 words
The process of claim 51, wherein the pH is from about 9 to about 11.
Claim 57
Dependent Claim
16 words
The process of claim 51 or 52 wherein the aqueous solution is comprised of sodium hydroxide.
Claim 58
Dependent Claim
18 words
A process for the filtration of fluids comprising passing the fluid through the microporous membrane of claim 1.
Claim 59
Dependent Claim
21 words
A process for the filtration of parenteral or body liquids comprising passing the liquids through the microporous membrane of claim 1.
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