IP Library Granted Patent US 7,462,666
Granted Patent B2
US 7,462,666 · App. 10/843,228 · Granted Dec 9, 2008

Method for making nanocomposite materials

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Quick Facts
Patent No.
US 7,462,666
App. No.
10/843,228
Granted
Dec 9, 2008
Kind
B2
Abstract

A method for making a nanocomposite material includes introducing a solution including a nanofiller material and a supercritical fluid into a molten polymeric material within an extruder. The supercritical fluid is caused to substantially instantaneously convert to a gas phase, thereby forming the nanocomposite material having the nanofiller material substantially homogeneously dispersed therein.

Claims (51)

1. A method for making a nanocomposite material, the method comprising the steps of:

providing a molten polymeric material in an extruder;

introducing a solution including a nanofiller material and a supercritical fluid into a molten polymeric material; and

causing the supercritical fluid within the solution to substantially instantaneously convert to a gas phase, thereby forming the nanocomposite material having the nanofiller material substantially homogeneously dispersed therein.

2. The method as defined in claim 1 , further comprising the step of passing the nanocomposite material through the extruder.

3. The method as defined in claim 1 wherein the supercritical fluid comprises at least one of hydrogen, neon, n-pentane, nitrogen, carbon tetrafluoride, chlorotrifluoromethane, cyclohexane, toluene, propane, trichlorofluoromethane, methane, propylene, argon, trifluoromethane, ethane, chlorodifluoromethane, ethylene, oxygen, krypton, xenon, acetylene, nitrous oxide, carbon dioxide, ammonia, water, and mixtures thereof.

4. The method as defined in claim 1 wherein the supercritical fluid comprises at least one of carbon dioxide, nitrogen, carbon tetrafluoride, chlorotrifluoride, trichlorofluoromethane, argon, trifluoromethane, chlorodifluoromethane, and mixtures thereof.

5. The method as defined in claim 1 wherein the nanofiller material comprises a clay including at least one of smectite clay, an illite clay, and mixtures thereof.

6. The method as defined in claim 1 wherein the supercritical fluid expands the nanofiller material by increasing a distance between at least two layers in the nanofiller material.

7. The method as defined in claim 1 wherein the solution has a nanofiller material concentration ranging between about 1 wt. % and about 50 wt. %.

8. The method as defined in claim 1 wherein the introducing step is accomplished by injecting the solution directly into the molten polymeric material.

9. The method as defined in claim 8 wherein causing the supercritical fluid to substantially instantaneously convert to the gas phase is accomplished by releasing pressure within the extruder, thereby aiding in exfoliation of the nanofiller material.

10. The method as defined in claim 1 wherein the pressure is greater than about 1200 psig.

11. The method as defined in claim 1 wherein the molten polymeric material comprises thermoplastic materials.

12. The method as defined in claim 11 wherein the thermoplastic materials comprise at least one of thermoplastic olefins, polyamides, thermoplastic urethanes, polystyrenes, and mixtures thereof.

13. The method as defined in claim 12 wherein the thermoplastic olefins comprise at least one of polypropylenes, polypropylene homopolymers, ethylene-propylene elastomers, polyethylenes, elastomers, impact copolymers thereof, and mixtures thereof.

14. A method for making a nanocomposite material, the method comprising the steps of:

providing a molten polymeric material in an extruder;

introducing a solution including a nanofiller material and a supercritical fluid into a barrel of an extruder having a molten polymeric material therein;

causing the supercritical fluid within the solution to substantially instantaneously convert to a gas phase, thereby forming a powdered nanofiller material on the molten polymeric material; and

passing the molten polymeric material having the powdered nanofiller material thereon through the extruder, thereby forming the nanocomposite material having the nanofiller material substantially homogeneously dispersed therein.

15. The method as defined in claim 14 wherein causing the supercritical fluid to substantially instantaneously convert to the gas phase is accomplished by releasing pressure within the extruder substantially upon introduction.

16. The method as defined in claim 14 wherein a space is defined between the molten polymeric material and an inside wall of the barrel, and wherein the solution is introduced into the space.

17. The method as defined in claim 14 wherein the molten polymeric material comprises a thermoplastic material comprising at least one of thermoplastic olefins, polyamides, thermoplastic urethanes, polystyrenes, and mixtures thereof.

18. The method as defined in claim 17 wherein the thermoplastic olefins comprise at least one of polypropylenes, polypropylene homopolymers, ethylene-propylene elastomers, polyethylenes, elastomers, impact copolymers thereof, and mixtures thereof.

19. The method as defined in claim 14 wherein the supercritical fluid comprises at least one of hydrogen, neon, n-pentane, nitrogen, carbon tetrafluoride, chlorotrifluoromethane, cyclohexane, toluene, propane, trichlorofluoromethane, methane, propylene, argon, trifluoromethane, ethane, chlorodifluoromethane, ethylene, oxygen, krypton, xenon, acetylene, nitrous oxide, carbon dioxide, ammonia, water, and mixtures thereof.

20. The method as defined in claim 14 wherein the supercritical fluid comprises at least one of carbon dioxide, nitrogen, carbon tetrafluoride, chlorotrifluoride, trichlorofluoromethane, argon, trifluoromethane, chlorodifluoromethane, and mixtures thereof.

21. The method as defined in claim 14 wherein the nanofiller material comprises a clay is selected from a smectite clay, and mixtures thereof.

22. A method for making a nanocomposite material, the method comprising the steps of:

preparing a solution having a nanofiller material and a supercritical fluid therein;

introducing a polymeric material into an extruder, wherein the polymeric material becomes molten downstream in the extruder;

injecting the solution into the molten polymeric material; and

releasing pressure in the extruder, thereby causing the supercritical fluid to substantially instantaneously convert to a gas phase, wherein the nanocomposite material having the nanofiller material substantially homogeneously dispersed therein is formed, and wherein the gas phase aids in exfoliation of the nanofiller material.

23. The method as defined in claim 22 wherein the polymeric material is fed into an upstream end of the extruder.

24. The method as defined in claim 22 wherein the polymeric material is fed into the extruder at a rate rangeing between about 50 lbs/hour and about 10,000 lbs/hour.

25. The method as defined in claim 22 wherein the polymeric material comprises a thermoplastic material comprising at least one of thermoplastic olefins, polyamides, thermoplastic urethanes, polystyrenes, and mixtures thereof.

26. The method as defined in claim 22 wherein the supercritical fluid comprises at least one of hydrogen, neon, n-pentane, nitrogen, carbon tetrafluoride, chlorotrifluoromethane, cyclohexane, toluene, propane, trichlorofluoromethane, methane, propylene, argon, trifluoromethane, ethane, chlorodifluoromethane, ethylene, oxygen, krypton, xenon, acetylene, nitrous oxide, carbon dioxide, ammonia, water, and mixtures thereof.

27. The method as defined in claim 22 wherein the supercritical fluid comprises at least one of carbon dioxide, nitrogen, carbon tetrafluoride, chlorotrifluoride, trichlorofluoromethane, argon, trifluoromethane, chlorodifluoromethane, and mixtures thereof.

28. A method for making a nanocomposite material, the method comprising the steps of:

preparing a supercritical solution having a nanofiller material and solvent therein;

introducing a polymeric material into an extruder, wherein the polymeric material becomes molten downstream in the extruder;

injecting the supercritical solution into a space within a barrel of the extruder, the space being defined between the molten polymeric material and an inside wall of the barrel;

releasing pressure in the extruder, thereby forming a finely divided, powdered nanofiller material on the molten polymeric material; and

passing the molten polymeric material having the powdered nanofiller material thereon through remaining sections of the extruder, thereby forming the nanocomposite material having the nanofiller material substantially homogeneously dispersed therein.

29. The method as defined in claim 28 wherein the supercritical fluid comprises at least one of hydrogen, neon, n-pentane, nitrogen, carbon tetrafluoride, chlorotrifluoromethane, cyclohexane, toluene, propane, trichlorofluoromethane, methane, propylene, argon, trifluoromethane, ethane, chlorodifluoromethane, ethylene, oxygen, krypton, xenon, acetylene, nitrous oxide, carbon dioxide, ammonia, water, and mixtures thereof.

30. The method as defined in claim 28 wherein the solvent is a supercritical fluid comprising at least one of carbon dioxide, nitrogen, carbon tetrafluoride, chlorotrifluoride, trichlorofluoromethane, argon, trifluoromethane, chlorodifluoromethane, and mixtures thereof.

31. The method as defined in claim 28 wherein the nanofiller material comprises a clay selected from a smectite clay, an illite clay, and mixtures thereof.

32. The method as defined in claim 28 wherein the injecting and releasing occur substantially simultaneously.

33. The method as defined in claim 5 wherein the smectite clay is selected from hectorite, montmorillonite, bentonite, beidelite, saponite, stevensite, sauconite, nontronite, and mixtures thereof.

34. The method as defined in claim 21 wherein the smectite clay is selected from hectorite, montmorillonite, bentonite, beidelite, saponite, stevensite, sauconite, nontronite, and mixtures thereof.

35. The method as defined in claim 31 wherein the smectite clay is selected from hectorite, montmorillonite, bentonite, beidelite, saponite, stevensite, sauconite, nontronite, and mixtures thereof.

Assignments (13)
RELEASE OF SECURITY INTEREST Recorded Nov 7, 2014
From: WILMINGTON TRUST COMPANY
To: GM GLOBAL TECHNOLOGY OPERATIONS LLC
Reel/Frame 034371/0676 →
CHANGE OF NAME Recorded Feb 10, 2011
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: GM GLOBAL TECHNOLOGY OPERATIONS LLC
Reel/Frame 025780/0902 →
SECURITY AGREEMENT Recorded Nov 8, 2010
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: WILMINGTON TRUST COMPANY
Reel/Frame 025327/0001 →
RELEASE OF SECURITY INTEREST Recorded Nov 4, 2010
From: UNITED STATES DEPARTMENT OF THE TREASURY
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 025245/0442 →
RELEASE OF SECURITY INTEREST Recorded Nov 4, 2010
From: UAW RETIREE MEDICAL BENEFITS TRUST
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 025311/0770 →
SECURITY AGREEMENT Recorded Aug 28, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: UAW RETIREE MEDICAL BENEFITS TRUST
Reel/Frame 023162/0001 →
SECURITY AGREEMENT Recorded Aug 27, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: UNITED STATES DEPARTMENT OF THE TREASURY
Reel/Frame 023156/0052 →
RELEASE OF SECURITY INTEREST Recorded Aug 21, 2009
From: CITICORP USA, INC. AS AGENT FOR BANK PRIORITY SECURED PARTIES; CITICORP USA, INC. AS AGENT FOR HEDGE PRIORITY SECURED PARTIES
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 023127/0468 →
RELEASE OF SECURITY INTEREST Recorded Aug 20, 2009
From: UNITED STATES DEPARTMENT OF THE TREASURY
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 023124/0429 →
SECURITY AGREEMENT Recorded Apr 16, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: CITICORP USA, INC. AS AGENT FOR BANK PRIORITY SECURED PARTIES; CITICORP USA, INC. AS AGENT FOR HEDGE PRIORITY SECURED PARTIES
Reel/Frame 022553/0446 →
SECURITY AGREEMENT Recorded Feb 4, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: UNITED STATES DEPARTMENT OF THE TREASURY
Reel/Frame 022201/0610 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 14, 2009
From: GENERAL MOTORS CORPORATION
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 022102/0533 →
CORRECTIVE ASSIGNMENT TO RE-RECORD ASSIGNMENT PREVIOUSLY RECORDED UNDER REEL AND FRAME 014909/0148 TO CORRECT THE SERIAL NUMBER FROM 10834228 TO 10843228. Recorded Sep 21, 2004
From: OTTAVIANI, ROBERT AUGUSTINE; RODGERS, WILLIAM R.; FASULO, PAULA D.; OKONSKI, DAVID A.
To: GENERAL MOTORS CORPORATION
Reel/Frame 015153/0536 →