US5698624A — Exfoliated layered materials and nanocomposites c…

Claim 1

Independent Claim 148 words

A composite material comprising a matrix polymer in an amount of about 40% to about 99.95% by weight of the composite material, and about 0.05% to about 60% by weight exfoliated platelets of a phyllosilicate material, said platelets derived from an intercalate formed by contacting a phyllosilicate with a water-insoluble intercalant polymer-containing composition, without first reacting the phyllosilicate with an onium ion or silane coupling agent, said composition having a concentration of said intercalant polymer of at least about 2% by weight polymer, wherein the amount of intercalant polymer in said composition comprises at least about 15% by weight, based on the weight of the phyllosilicate contacted, to achieve sorption of the water-insoluble intercalant polymer between adjacent spaced layers of the phyllosilicate to expand the spacing between a predominance of the adjacent phyllosilicate platelets to at least about 10 Å, when measured after sorption of the water-insoluble polymer.

Claim 2

Dependent Claim 148 words

A composite material comprising a matrix polymer in an amount of about 40% to about 99.95% by weight of the composite material, and about 0.05% to about 60% by weight exfoliated platelets of a phyllosilicate material, said platelets derived from an intercalate formed by contacting a phyllosilicate with a water-insoluble intercalant polymer-containing composition, without first reacting the phyllosilicate with an onium ion or silane coupling agent, said composition having a concentration of said intercalant polymer of at least about 2% by weight polymer, wherein the amount of intercalant polymer in said composition comprises at least about 15% by weight, based on the weight of the phyllosilicate contacted, to achieve sorption of the water-insoluble intercalant polymer between adjacent spaced layers of the phyllosilicate to expand the spacing between a predominance of the adjacent phyllosilicate platelets to at least about 10 Å, when measured after sorption of the water-insoluble polymer.

Claim 3

Dependent Claim 26 words

A composite material in accordance with claim 1, wherein the concentration of water-insoluble intercalant polymer in said phyllosilicate-contacting composition is at least about 5% by weight.

Claim 4

Dependent Claim 26 words

A composite material in accordance with claim 2, wherein the concentration of water-insoluble intercalant polymer in said phyllosilicate-contacting composition is at least about 15% by weight.

Claim 5

Dependent Claim 26 words

A composite material in accordance with claim 3, wherein the concentration of water-insoluble intercalant polymer in said phyllosilicate-contacting composition is at least about 20% by weight.

Claim 6

Dependent Claim 26 words

A composite material in accordance with claim 4, wherein the concentration of water-insoluble intercalant polymer in said phyllosilicate-contacting composition is at least about 30% by weight.

Claim 7

Dependent Claim 30 words

A composite material in accordance with claim 5, wherein the concentration of water-insoluble intercalant polymer in said phyllosilicate-contacting composition in the range of about 50% to about 80% by weight.

Claim 8

Dependent Claim 30 words

A composite material in accordance with claim 5, wherein the concentration of water-insoluble intercalant polymer in said phyllosilicate-contacting composition in the range of about 50% to about 100% by weight.

Claim 9

Dependent Claim 36 words

A composite material in accordance with claim 1, wherein the concentration of water-insoluble intercalant polymer in the phyllosilicate-contacting composition is initially at least about 16% by weight, based on the dry weight of the phyllosilicate contacted.

Claim 10

Dependent Claim 40 words

A composite material in accordance with claim 8, wherein the concentration of intercalant polymer in the phyllosilicate-contacting composition is initially in the range of about 16% to about 70% by weight, based on the dry weight of the phyllosilicate contacted.

Claim 11

Dependent Claim 42 words

A composite material in accordance with claim 9, wherein the concentration of intercalant polymer in the phyllosilicate-contacting composition is initially in the range of about 16% to less than about 35% by weight, based on the dry weight of the phyllosilicate contacted.

Claim 12

Dependent Claim 42 words

A composite material in accordance with claim 9, wherein the concentration of intercalant polymer in the phyllosilicate-contacting composition is initially in the range of about 35% to less than about 55% by weight, based on the dry weight of the phyllosilicate contacted.

Claim 13

Dependent Claim 32 words

A composite material in accordance with claim 9, wherein the concentration of the intercalant polymer in the phyllosilicate-contacting composition is 70% by weight, based on the dry weight of the phyllosilicate contacted.

Claim 14

Dependent Claim 27 words

A composite material in accordance with claim 1, wherein the intercalant polymer has a weight average molecular weight in the range of about 225 to about 1,000,000.

Claim 15

Dependent Claim 27 words

A composite material in accordance with claim 13, wherein the intercalant polymer has a weight average molecular weight in the range of about 225 to about 10,000.

Claim 16

Dependent Claim 47 words

A composite material in accordance with claim 1, wherein the matrix polymer is selected from the group consisting of a polyamide; polyvinylimine; polyethylene terephthalate; polybutylene terephthalate; a polymer polymerized from a monomer selected from the group consisting of dihydroxyethyl terephthalate; hydroxyethyl terephthalate; dihydroxybutyl terephthalate; and mixtures thereof.

Claim 17

Independent Claim 199 words

A method of manufacturing a composite material containing about 40% to about 99.95% by weight of a matrix thermoplastic or thermosetting polymer, and about 0.05% to about 60% by weight of exfoliated platelets of a phyllosilicate material, said platelets derived from an intercalated phyllosilicate having a water-insoluble polymer intercalated between adjacent phyllosilicate platelets comprising: contacting the phyllosilicate with an intercalant polymer-containing composition without first reacting the phyllosilicate with an onium ion or silane coupling agent, said composition comprising at least about 5% by weight of a water-insoluble polymer, having a water-solubility of less than about 5 grams polymer per 100 milliliters of distilled water, at 25° C., wherein the amount of intercalant polymer in said composition comprises at least about 15% by weight, based on the weight of the phyllosilicate contacted, to achieve intercalation of said polymer between said adjacent phyllosilicate platelets in an amount sufficient to space said adjacent phyllosilicate platelets a distance of at least about 10 Å; combining the intercalated platelets with said thermoplastic polymer, and heating the thermoplastic polymer sufficiently to provide for flow of said thermoplastic polymer and delamination of the platelets of said phyllosilicate; and dispersing said delaminated platelets throughout said matrix polymer.

Claim 18

Independent Claim 199 words

A method of manufacturing a composite material containing about 40% to about 99.95% by weight of a matrix thermoplastic or thermosetting polymer, and about 0.05% to about 60% by weight of exfoliated platelets of a phyllosilicate material, said platelets derived from an intercalated phyllosilicate having a water-insoluble polymer intercalated between adjacent phyllosilicate platelets comprising: contacting the phyllosilicate with an intercalant polymer-containing composition without first reacting the phyllosilicate with an onium ion or silane coupling agent, said composition comprising at least about 5% by weight of a water-insoluble polymer, having a water-solubility of less than about 5 grams polymer per 100 milliliters of distilled water, at 25° C., wherein the amount of intercalant polymer in said composition comprises at least about 15% by weight, based on the weight of the phyllosilicate contacted, to achieve intercalation of said polymer between said adjacent phyllosilicate platelets in an amount sufficient to space said adjacent phyllosilicate platelets a distance of at least about 10 Å; combining the intercalated platelets with said thermoplastic polymer, and heating the thermoplastic polymer sufficiently to provide for flow of said thermoplastic polymer and delamination of the platelets of said phyllosilicate; and dispersing said delaminated platelets throughout said matrix polymer.

Claim 19

Dependent Claim 36 words

The method of claim 16, wherein said intercalant polymer-containing composition includes a dissolved polymer carrier comprising about 5% to about 95% by weight organic solvent, based on the total weight of said composition contacting said phyllosilicate.

Claim 20

Dependent Claim 18 words

The method of claim 17, wherein said carrier comprises about 5% to about 95% of an aliphatic alcohol.

Claim 21

Dependent Claim 20 words

The method of claim 18, wherein said alcohol is selected from the group consisting of methanol, ethanol, and mixtures thereof.

Claim 22

Dependent Claim 151 words

A composite material comprising a matrix polymer in an amount of about 40% to about 99.95% by weight of the composite material, and about 0.05% to about 60% by weight exfoliated platelets of a phyllosilicate material, said platelets derived from an intercalate formed by contacting a phyllosilicate with a water-insoluble intercalant polymer-containing composition, without a coupling agent selected from the group consisting of onium ion and silane coupling agents, said composition having a concentration of said water-insoluble intercalant polymer of at least about 2% by weight polymer, and in a quantity sufficient to incorporate a layer of water-insoluble polymer between adjacent phyllosilicate platelets of sufficient thickness for exfoliation of said platelets, to achieve sorption of the intercalant polymer between adjacent spaced layers of the phyllosilicate to expand the spacing between a predominance of the adjacent phyllosilicate platelets to at least about 10 Å, when measured after sorption of the intercalant polymer.

Claim 23

Dependent Claim 151 words

A composite material comprising a matrix polymer in an amount of about 40% to about 99.95% by weight of the composite material, and about 0.05% to about 60% by weight exfoliated platelets of a phyllosilicate material, said platelets derived from an intercalate formed by contacting a phyllosilicate with a water-insoluble intercalant polymer-containing composition, without a coupling agent selected from the group consisting of onium ion and silane coupling agents, said composition having a concentration of said water-insoluble intercalant polymer of at least about 2% by weight polymer, and in a quantity sufficient to incorporate a layer of water-insoluble polymer between adjacent phyllosilicate platelets of sufficient thickness for exfoliation of said platelets, to achieve sorption of the intercalant polymer between adjacent spaced layers of the phyllosilicate to expand the spacing between a predominance of the adjacent phyllosilicate platelets to at least about 10 Å, when measured after sorption of the intercalant polymer.

Claim 24

Dependent Claim 39 words

A composite material in accordance with claim 20, wherein the quantity of intercalant polymer in said intercalant polymer-containing composition is about 16% to about 80% by weight, based on the weight of phyllosilicate contacted by said intercalant polymer-containing composition.

Claim 25

Independent Claim 199 words

A method of manufacturing a composite material containing about 40% to about 99.95% by weight of a matrix thermoplastic or thermosetting polymer, and about 0.05% to about 60% by weight of exfoliated platelets of a phyllosilicate material, said platelets derived from an intercalated phyllosilicate having a water-insoluble polymer intercalated between adjacent phyllosilicate platelets comprising: contacting the phyllosilicate with an intercalant polymer-containing composition, without a coupling agent selected from the group consisting of onium ion and silane coupling agents, comprising at least about 5% by weight of a water-insoluble polymer, having a water-solubility of less than about 5 grams polymer per 100 milliliters of distilled water, at 25° C., and in a quantity sufficient to incorporate a layer of polymer between adjacent phyllosilicate platelets of sufficient thickness for exfoliation of said platelets, to achieve intercalation of said polymer between said adjacent phyllosilicate platelets in an amount sufficient to space said adjacent phyllosilicate platelets a distance of at least about 10 Å; combining the intercalated platelets with said thermoplastic polymer, and heating the thermoplastic polymer sufficiently to provide for flow of said thermoplastic polymer and delamination of the platelets of said phyllosilicate; and dispersing said delaminated platelets throughout said matrix polymer.

Claim 26

Independent Claim 199 words

A method of manufacturing a composite material containing about 40% to about 99.95% by weight of a matrix thermoplastic or thermosetting polymer, and about 0.05% to about 60% by weight of exfoliated platelets of a phyllosilicate material, said platelets derived from an intercalated phyllosilicate having a water-insoluble polymer intercalated between adjacent phyllosilicate platelets comprising: contacting the phyllosilicate with an intercalant polymer-containing composition, without a coupling agent selected from the group consisting of onium ion and silane coupling agents, comprising at least about 5% by weight of a water-insoluble polymer, having a water-solubility of less than about 5 grams polymer per 100 milliliters of distilled water, at 25° C., and in a quantity sufficient to incorporate a layer of polymer between adjacent phyllosilicate platelets of sufficient thickness for exfoliation of said platelets, to achieve intercalation of said polymer between said adjacent phyllosilicate platelets in an amount sufficient to space said adjacent phyllosilicate platelets a distance of at least about 10 Å; combining the intercalated platelets with said thermoplastic polymer, and heating the thermoplastic polymer sufficiently to provide for flow of said thermoplastic polymer and delamination of the platelets of said phyllosilicate; and dispersing said delaminated platelets throughout said matrix polymer.

Claim 27

Dependent Claim 38 words

A method in accordance with claim 22, wherein the quantity of intercalant polymer in said intercalant polymer-containing composition is about 16% to about 80% by weight, based on the weight of phyllosilicate contacted by said intercalant polymer-containing composition.

Claim 28

Dependent Claim 30 words

A composite material in accordance with claim 1, wherein the amount of polymer intercalated into the phyllosilicate material is 10-90% polymer based on the dry weight of the phyllosilicate material.

Claim 29

Dependent Claim 33 words

A composite material in accordance with claim 24, wherein the amount of polymer intercalated into the phyllosilicate material is about 15% to about 80%, based on the dry weight of the phyllosilicate material.

Claim 30

Dependent Claim 43 words

A composite material in accordance with claim 25, wherein the weight ratio of intercalated polymer to phyllosilicate material is from about 16 grams of polymer per 100 grams of phyllosilicate material to about 80 grams of polymer per 100 grams of phyllosilicate material.

Claim 31

Dependent Claim 43 words

A composite material in accordance with claim 26, wherein the weight ratio of intercalated polymer to phyllosilicate material is from about 20 grams of polymer per 100 grams of phyllosilicate material to about 60 grams of polymer per 100 grams of phyllosilicate material.

Claim 32

Dependent Claim 30 words

A composite material in accordance with claim 1, wherein the weight ratio of intercalant polymer to phyllosilicate material in the intercalating composition is in the range of 1:20 to 1:3.

Claim 33

Dependent Claim 29 words

A method in accordance with claim 16, wherein the amount of polymer intercalated into the phyllosilicate material is 10-90% polymer, based on the dry weight of the phyllosilicate material.

Claim 34

Dependent Claim 32 words

A method in accordance with claim 29, wherein the amount of polymer intercalated into the phyllosilicate material is about 15% to about 80%, based on the dry weight of the phyllosilicate material.

Claim 35

Dependent Claim 42 words

A method in accordance with claim 30, wherein the weight ratio of intercalated polymer to phyllosilicate material is from about 16 grams of polymer per 100 grams of phyllosilicate material to about 80 grams of polymer per 100 grams of phyllosilicate material.

Claim 36

Dependent Claim 42 words

A method in accordance with claim 31, wherein the weight ratio of intercalated polymer to phyllosilicate material is from about 20 grams of polymer per 100 grams of phyllosilicate material to about 60 grams of polymer per 100 grams of phyllosilicate material.

Claim 37

Dependent Claim 30 words

A method in accordance with claim 16, wherein the weight ratio of intercalant polymer to phyllosilicate material in the intercalant polymer-containing composition is in the range of 1:20 to 1:3.

Claim 38

Dependent Claim 30 words

A composite material in accordance with claim 20, wherein the amount of polymer intercalated into the phyllosilicate material is 10-90% polymer, based on the dry weight of the phyllosilicate material.

Claim 39

Dependent Claim 30 words

A composite material in accordance with claim 34, wherein the amount of polymer intercalated into the phyllosilicate material is 15-80% polymer, based on the dry weight of the phyllosilicate material.

Claim 40

Dependent Claim 43 words

A composite material in accordance with claim 35, wherein the weight ratio of intercalated polymer to phyllosilicate material is from about 16 grams of polymer per 100 grams of phyllosilicate material to about 80 grams of polymer per 100 grams of phyllosilicate material.

Claim 41

Dependent Claim 31 words

A composite material in accordance with claim 20, wherein the weight ratio of intercalant polymer to phyllosilicate material in the intercalant polymer-containing composition is in the range of 1:20 to 1:3.

Claim 42

Dependent Claim 29 words

A method in accordance with claim 22, wherein the amount of polymer intercalated into the phyllosilicate material is 10-90% polymer, based on the dry weight of the phyllosilicate material.

Claim 43

Dependent Claim 33 words

A method in accordance with claim 38, wherein the amount of polymer intercalated into the phyllosilicate material is about 15% to about 80% polymer, based on the dry weight of the phyllosilicate material.

Claim 44

Dependent Claim 42 words

A method in accordance with claim 39, wherein the weight ratio of intercalated polymer to phyllosilicate material is from about 16 grams of polymer per 100 grams of phyllosilicate material to about 80 grams of polymer per 100 grams of phyllosilicate material.

Claim 45

Dependent Claim 42 words

A method in accordance with claim 40, wherein the weight ratio of intercalated polymer to phyllosilicate material is from about 20 grams of polymer per 100 grams of phyllosilicate material to about 60 grams of polymer per 100 grams of phyllosilicate material.

Claim 46

Dependent Claim 29 words

A method in accordance with claim 22, wherein the weight ratio of intercalant polymer to phyllosilicate in the intercalant polymer-containing composition is in the range of 1:20 to 1:3.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	2000-12-15	2001-06-16	2001-12-16	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	2004-12-15	2005-06-16	2005-12-16	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	2008-12-15	2009-06-16	2009-12-16	$7700.00	Window Closed / Lapsed

Exfoliated layered materials and nanocomposites comprising matrix polymers and said exfoliated layered materials formed with water-insoluble oligomers and polymers

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