IP Library Granted Patent US 8,481,616
Granted Patent B2
US 8,481,616 · App. 13/351,004 · Granted Jul 9, 2013

Intercalation agent free compositions useful to make nanocomposite polymers

Inventors: Luyi Sun (Bryan, TX); Jae Woong Boo (College Station, TX); Hung-jue Sue (College Station, TX); Maurice J. Marks (Lake Jackson, TX); Richard F. Fibiger (Midland, MI); Michael S. Paquette (Midland, MI)
Assignees: Dow Global Technologies LLC; The Texas A & M University
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 8,481,616
App. No.
13/351,004
Granted
Jul 9, 2013
Kind
B2
Abstract

A two step method for preparing a filler composition, the filler composition useful to prepare a nanocomposite polymer and an epoxy nanocomposite coating. First, disperse a water dispersible filler material in a liquid comprising water, but without any added intercalation agent, to form a dispersion. Second, replace at least a portion of the water of the liquid with an organic solvent so that the water concentration of the liquid is less than six percent by weight to form the filler composition, the average size of at least one dimension of the filler material being less than two hundred nanometers upon examination by transmission electron microscopy of a representative freeze dried sample of the dispersion of the first step. A nanocomposite polymer can be prepared by mixing the filler composition with one or more polymer, polymer component, monomer or prepolymer to produce a polymer containing the filler composition.

Claims (22)

1. A filler composition formed by:

(1) dispersing a water dispersible filler material in a liquid comprising water; and

(2) replacing most of the water of the liquid with an organic solvent so that the water concentration of the liquid is less than six percent by weight to form the filler composition, the average size of at least one dimension of the filler material being less than two hundred nanometers upon examination by transmission electron microscopy of a representative freeze dried sample of the dispersion of (1);

wherein the filler composition is formed without adding an intercalation agent to the water dispersible filler material, and the water dispersible filler material is a cation exchanging layered material having a cation exchanging capacity that is less than twenty percent exchanged with an organic cation.

2. The filler composition of claim 1 , wherein the cation exchanging layered material is selected from the group consisting of natural or synthetic bentonite, montmorillonite, hectorite, fluorohectorite, saponite, stevensite, nontronite, sauconite, glauconite, vermiculite, chlorite, mica, hydromica, muscovite, biotite, phlogopite, illite, talc, pyrophillite, sepiolite, attapulgite, palygorskite, berthierine, serpentine, kaolinite, dickite, nacrite, halloysite, allophane, immogolite, hydrotalcite, pyroaurite, calcite, wollastonite and mixtures thereof.

3. The filler composition of claim 1 , wherein the water concentration of the liquid is less than three percent by weight.

4. The filler composition of claim 1 , wherein the water concentration of the liquid is less than one percent by weight.

5. The filler composition of claim 1 , wherein the water concentration of the liquid is less than one half percent by weight.

6. The filler composition of claim 1 , wherein the water concentration of the liquid is less than one tenth percent by weight.

7. A nanocomposite polymer, made by the steps of:

providing the filler composition of claim 1 ; and

mixing the filler composition with one or more polymer, polymer component, monomer or prepolymer to produce the nanocomposite polymer containing the filler composition.

8. The nanocomposite polymer of claim 7 , wherein the polymer is selected from the group consisting of polymers and copolymers of, polyolefins, polyamids, polyesters, polycarbonates, epoxies, styrenic polymers, polyurethanes, poly(alkyl)acrylates, polyacetals, polysulfides, polysulfones, polyethers, polyarylethers, polyketones, polyarylketones, polyimides, poly(vinyl halide)s, poly(vinylidene halide)s, poly(tetrafluoroethylene), polysiloxanes, cyanate polymers, maleimide polymers, vinylester resin polymers and mixtures thereof.

9. The nanocomposite polymer of claim 7 , wherein the monomer comprises an epoxy resin and wherein the filler composition is mixed with the epoxy resin to form an epoxy resin mixture, where the epoxy resin mixture is devolatilized to remove organic solvent.

10. The nanocomposite polymer of claim 9 , further including an epoxy resin curing agent mixed with the epoxy resin mixture to produce a cured epoxy nanocomposite polymer containing filler having an average size of at least one dimension of the filler of less than two hundred nanometers upon examination by transmission electron microscopy of a representative sample of the cured epoxy nanocomposite polymer.

11. An epoxy nanocomposite coating made by the steps of:

(a) providing the filler composition of claim 1 :

(b) mixing an epoxy resin with the filler composition;

(c) mixing a curing agent and optionally a catalyst, accelerator, and processing additives with the epoxy resin and the filler composition to form a mixture;

(d) applying the mixture to a substrate; and

(e) allowing the organic solvent in the mixture to evaporate and the mixture to cure.

12. The epoxy nanocomposite coating of claim 11 , including exchanging and/or adding organic solvents after steps (b) or (c).

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2015
From: DOW GLOBAL TECHNOLOGIES LLC
To: BLUE CUBE IP LLC
Reel/Frame 035873/0984 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 23, 2014
From: MARKS, MAURICE J.; FIBIGER, RICHARD F.; PAQUETTE, MICHAEL S.
To: DOW GLOBAL TECHNOLOGIES LLC
Reel/Frame 033154/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 23, 2014
From: SUN, LUYI; SUE, HUNG-JUE; BOO, WOONG JAE
To: THE TEXAS A&M UNIVERSITY
Reel/Frame 033154/0020 →
Continuity (3)
Continuation 12515692
Provisional Application 60861872 · Nov 30, 2006
Related Publication 20120136093A1 · May 31, 2012