Mesoporous materials and methods of making the same

• US 6,696,258 B1
• Filed: 06/21/2000
• Issued: 02/24/2004
• Est. Priority Date: 01/20/1998
• Status: Expired due to Fees

• Current Assignee: Drexel University
• Original Assignee: Drexel University
• Inventors: Jin, Danliang, Xu, Jigeng, Wei, Yen, Ding, Tianzhong
• Primary Examiner(s): Le, Long V.
• Assistant Examiner(s): Padmanabhan, Kartic
• Application Number:
  US09/598,717
• Time in Patent Office: 1,343 Days
• Field of Search: 423/702, 424/484, 424/489, 424/499, 435/4, 435/7.1, 435/7.2, 435/14, 436/518, 436/523, 436/524, 436/528
• US Class Current: 435/7.2
• CPC Class Codes: A61K 9/143 with inorganic compounds
• CPC Class Codes: C01B 37/02 Crystalline silica-polymorphs, e.g. silicalites dealuminated aluminosilicate zeolites

Abstract

Mesoporous materials and a method for making such materials is disclosed in which the mesoporous materials are made by forming an aqueous solution having an organometallic compound; adding a solution comprising a pore forming material selected from the group consisting of monomeric polyols, polyacids, polyamines, carbohydrates, oligopeptides, oligonucleic acids, carbonyl functional organic compounds, and mixtures and derivatives of these materials to form a sol get matrix by polycondensation; drying the sot gel matrix; and removing the pore forming material from the dried sot-gel matrix to thereby form a mesoporous material. The mesoporous materials have pore diameters of from about 20 Å to about 100 Å and may be used with a biologically active agent immobilized within the pores of the mesoporous material and introduced into a biological system.

Claims

1. A method for making a mesoporous material comprising:

(a) forming an aqueous solution having an organometallic compound;

(b) adding a solution to the aqueous solution, the added solution comprising a pore forming material selected from the group consisting of monomeric polyols, polyacids, polyamines, carbohydrates, oligopeptides of at least two amino acid units, oligonucleic acids, carbonyl functional organic compounds, and mixtures and derivatives thereof to form a sol gel matrix by polycondensation;

(c) drying the sol gel matrix; and

(d) removing the pore forming material from the dried sol-gel matrix to thereby form a mesoporous material.

2. The method of claim 1, wherein the mesoporous material is formed such that substantially all pores are mesopores, a mixture of mesopores and micropores, or a mixture of mesopores and macropores.

3. The method according to claim 1, wherein the pore forming material interacts by polar or hydrogen bonding with intermediates of the organometallic compound in the sol-gel matrix.

4. The method according to claim 1, wherein step (a) further comprises forming the aqueous solution having the organometallic compound by hydrolyzing at least one metal alkoxide.

5. The method according to claim 4, wherein the at least one metal alkoxide is selected from the group consisting of tetramethylorthosilicate and tetraethylorthosilicate.

6. The method according to claim 4, further comprising hydrolyzing that is acid catalyzed.

7. The method according to claim 6, further comprising hydrolyzing that is acid catalyzed using hydrochloric acid as an acid catalyst.

8. The method according to claim 4, further comprising hydrolyzing that is base catalyzed.

9. The method according to claim 8, further comprising hydrolyzing that is base catalyzed using sodium hydroxide as a base catalyst.

10. The method according to claim 1, wherein the pore forming material is a non-surfactant, polar compound which forms a hydrogen bond in the sol-gel matrix.

11. The method according to claim 1, wherein the pore forming material is selected from the group consisting of D-glucose, D-maltose, D-fructose, sucrose, dibenzoyl-L-tartaric acid, cyclodextrins, and soluble starches.

12. The method according to claim 1, wherein the mesoporous material has pores which are substantially all mesoporous and step (b) further comprises adding the pore forming material in an amount effective to provide an average pore diameter of from about 20 Å

to about 100 Å

in the mesoporous material.

13. The method according to claim 1, wherein step (b) further comprises adding at least 20% by weight of the pore forming material based on the weight of the dried sol-gel matrix.

14. The method according to claim 13, wherein the pore diameter is from about 30 Å

to about 60 Å

.

15. The method according to claim 1, wherein step (c) further comprises drying the sol gel matrix by evaporation to form a solid matrix.

16. The method according to claim 15, further comprising grinding the solid matrix prior to removing the pore forming material from the solid matrix.

17. The method according to claim 1, wherein step (d) further comprises removing the pore forming material from the solid matrix by solvent extraction or calcination.

18. The method according to claim 17, further comprising removing the pore forming material from the solid matrix by solvent extraction and extracting with water as a solvent.

19. The method according to claim 1, wherein step (b) further comprises adding a biologically active agent.

20. The method according to claim 19, wherein the biologically active agent is added in solution form after adding the solution comprising the pore forming material.

22. The method of claim 1, further comprising controlling degree of mesoporosity and average diameter of mesopores by varying a concentration of the pore forming material.

21. A method for making a mesoporous material comprising:

(a) forming an aqueous solution having an organometallic compound;

(b) adding a solution to the aqueous solution, the added solution comprising a pore forming material which is a non-surfactant to form a sol gel matrix by polycondensation;

(c) drying the sol gel matrix; and

(d) removing the pore forming material from the dried sol-gel matrix to thereby form a mesoporous material.