IP Library Granted Patent US 7,129,287
Granted Patent B1
US 7,129,287 · App. 10/425,565 · Granted Oct 31, 2006

Clay nanocomposites prepared by in-situ polymerization

Assignee: The Ohio State University
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Quick Facts
Patent No.
US 7,129,287
App. No.
10/425,565
Granted
Oct 31, 2006
Kind
B1
Abstract

A method for preparing exfoliated clay nanocomposites by in-situ polymerization comprising the steps of (a) providing a mixture of at least one type of monomer and at least one type of organophilic clay; and (b) initiating an in-situ polymerization reaction in the mixture so as to cause the at least one type of monomer to polymerize thereby forming the exfoliated clay nanocomposite. The exfoliated clay nanocomposite produces an x-ray diffraction pattern that is substantially devoid of an intercalation peak. The exfoliated clay nanocomposite may then be used as a masterbatch.

Claims (85)

1. A method for synthesizing 2-methacryloyloxyethylhexadecyldimethylammonium bromide, said method comprising the steps of:

reacting 2-(dimethylamino)ethyl methacrylate and 1-bromohexadecane in the presence of hydroquinone monomethyl ether so as to form a precipitate; and

purifying said precipitate so as to isolate said 2-methacryloyloxyethylhexadecyldimethylammonium bromide.

2. A compound having the formula:

wherein:

R1 is (CH 2 ) n wherein n ranges from 6 to 20;

R2 is a chemical structure having a terminal reactive double bond;

R3 is an alkyl group; and

R4 is an alkyl group.

3. The compound of claim 2 wherein n is 15, R3 is CH 3 , R 4 is CH 3 , and R2 is

4. A organophilic clay mixture, said organophilic clay mixture comprising:

a smectite clay; and

a compound having the formula:

wherein:

R1 is (CH 2 ) n wherein n ranges from 6 to 20;

R2 is a chemical structure having a terminal reactive double bond;

R3 is an alkyl group; and

R4 is an alkyl group.

5. The organophilic clay according to claim 4 wherein n is 15, R3 is CH 3 , R 4 is CH 3 , and R2 is:

6. The organophilic clay according to claim 4 wherein said smectite clay is selected from the group consisting of montmorillonite, hectorite, saponite, laponite, florohectorite, and beidellite.

7. A method for preparing an exfoliated clay nanocomposite by in-situ polymerization, said method comprising the steps of:

providing a mixture of at least one type of monomer and at least one type of organophilic clay mixture, said organophilic clay mixture comprising:

a compound having the formula:

wherein:

R1 is (CH 2 ) n wherein n ranges from 6 to 20;

R2 is a chemical structure having a terminal reactive double bond;

R3 is an alkyl group; and

R4 is an alkyl group; and

initiating an in-situ polymerization reaction in said mixture so as to cause said at least one type of monomer to polymerize thereby forming said exfoliated clay nanocomposite, said exfoliated clay nanocomposite producing an x-ray diffraction pattern substantially devoid of an intercalation peak.

8. The method according to claim 7 wherein said mixture comprises at least 15 weight percent of said organophilic clay.

9. The method according to claim 7 wherein said clay nanocomposite is an exfoliated nanocomposite having substantially uniform mesoscale clay dispersion.

10. The method according to claim 7 wherein said polymerization reaction is initiated by a chemical initiator.

11. The method according to claim 10 wherein said chemical initiator is selected from the group consisting of benzoyl peroxide and 2,2′-azobis(isobutyronitrile).

12. The method according to claim 7 wherein said organophilic clay comprises smectite clay selected from the group consisting of montmorillonite, hectorite, saponite, laponite, florohectorite, and beidellite.

13. The method according to claim 7 wherein said mixture additionally comprises at least one surfactant.

14. The method according to claim 7 at least one of said at least one monomer is selected from the group consisting of styrene, methyl methacrylate, ethylene, vinylene monomer, and mixtures thereof.

15. A clay nanocomposite prepared according to the method of claim 7 .

16. An exfoliated clay nanocomposite, said exfoliated clay nanocomposite comprising:

a polymeric portion; and

an organophilic clay portion, said organophilic clay portion dispersed throughout said polymeric portion such that an x-ray diffraction pattern produced from said exfoliated clay nanocomposite is substantially devoid of an intercalation peak, said organophilic clay portion comprising:

a compound having the formula:

wherein:

R1 is (CH 2 ) n wherein n ranges from 6 to 20;

R2 is a chemical structure having a terminal reactive double bond;

R3 is an alkyl group; and

R4 is an alkyl group.

17. The exfoliated clay nanocomposite according to claim 16 wherein said polymeric portion comprises a polymer selected from the group consisting of poly(methyl methacrylate), polystryrene, vinyl-based polymers, and mixtures thereof.

18. The exfoliated clay nanocomposite according to claim 16 wherein said organophilic clay comprises a smectite clay selected from the group consisting of montmorillonite, hectorite, saponite, laponite, florohectorite, and beidellite.

19. The exfoliated clay nanocomposite according to claim 16 wherein said wherein said clay nanocomposite is an exfoliated nanocomposite having a substantially uniform mesoscale clay dispersion.

20. The exfoliated clay nanocomposite according to claim 16 wherein said clay nanocomposite comprises at least 15 weight percent of said organophilic clay.

21. A method for producing an exfoliated clay nanocomposite-carrier resin mixture, said method comprising the steps of:

providing an exfoliated clay nanocomposite, said exfoliated clay nanocomposite comprising:

a polymeric portion; and

an organophilic clay portion, said organophilic clay portion dispersed throughout said polymeric portion such that an x-ray diffraction pattern produced from said exfoliated clay nanocomposite is substantially devoid of an intercalation peak, said organophilic clay mixture comprising:

a compound having the formula:

wherein:

R1 is (CH 2 ) n wherein n ranges from 6 to 20;

R2 is a chemical structure having a terminal reactive double bond;

R3 is an alkyl group; and

R4 is an alkyl group; and

blending said exfoliated clay nanocomposite with a carrier resin so as to substantially disperse said clay nanocomposite throughout said carrier resin thereby forming said exfoliated clay nanocomposite-carrier resin mixture.

22. The method according to claim 21 wherein said carrier resin is selected from the group consisting of polystyrene, poly(methyl methacrylate), vinyl-based polymers, and mixtures thereof.

23. The method according to claim 21 wherein said polymeric portion comprises a polymer selected from the group consisting of poly(methyl methacrylate), polystryrene, vinyl-based polymers, and mixtures thereof.

24. The method according to claim 21 wherein said organophilic clay comprises a smectite clay selected from the group consisting of montmorillonite, hectorite, saponite, laponite, florohectorite, and beidellite.

25. The method according to claim 21 wherein said clay nanocomposite is an exfoliated nanocomposite having a substantially uniform mesoscale clay dispersion.

26. The method according to claim 21 wherein said clay nanocomposite comprises at least 15 weight percent of said organophilic clay.

27. An exfoliated clay nanocomposite-carrier resin mixture prepared according to the method of claim 21 .

28. An exfoliated clay nanocomposite-carrier resin mixture, said mixture comprising:

a carrier resin; and

an exfoliated clay nanocomposite, said exfoliated clay nanocomposite substantially dispersed throughout said carrier resin, said exfoliated clay nanocomposite comprises:

a polymeric portion; and

an organophilic clay portion, said organophilic clay portion dispersed throughout said polymeric portion such that an x-ray diffraction pattern produced from said exfoliated clay nanocomposite is substantially devoid of an intercalation peak, said organophilic clay mixture comprising:

a compound having the formula:

wherein:

R1 is (CH 2 ) n wherein n ranges from 6 to 20;

R2 is a chemical structure having a terminal reactive double bond;

R3 is an alkyl croup; and

R4 is an alkyl group.

29. The exfoliated clay nanocomposite-carrier resin mixture of claim 28 wherein said carrier resin is selected from the group consisting of polystyrene, poly(methyl methacrylate), vinyl-based polymers, and mixtures thereof.

30. The exfoliated clay nanocomposite-carrier resin mixture according to claim 28 wherein said polymeric portion comprises a polymer selected from the group consisting of poly(methyl methacrylate), polystryrene, vinyl-based polymers, and mixtures thereof.

31. The exfoliated clay nanocomposite-carrier resin mixture according to claim 28 wherein said organophilic clay comprises smectite clay.

32. The exfoliated clay nanocomposite-carrier resin mixture according to claim 28 wherein said exfoliated clay nanocomposite has a substantially uniform mesoscale clay dispersion.

33. The exfoliated clay nanocomposite-carrier resin mixture according to claim 28 wherein said clay nanocomposite comprises at least 15 weight percent of said organophilic clay.

34. An article comprising said exfoliated clay nanocomposite-carrier resin mixture of claim 28 .

35. The exfoliated clay nanocomposite-carrier resin mixture according to claim 31 wherein said smectite clay is selected from the group consisting of montmorillonite, hectorite, saponite, laponite, florohectorite, and beidellite.

Assignments (1)
CONFIRMATORY LICENSE Recorded Jan 3, 2011
From: THE OHIO STATE UNIVERSITY RESEARCH FOUNDATION
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 025574/0365 →
Continuity (1)
Provisional Application 6037636500 · Apr 29, 2002