IP Library › Granted Patent US 11,096,911
Granted Patent B2
US 11,096,911 · App. 16/138,591 · Granted Aug 24, 2021

Hierarchical siliceous mesosilicalite nanocarrier

Inventors: B. Rabindran Jermy (Dammam, SA); Vijaya Ravinayagam (Dammam, SA)
Assignee: Imam Abdulrahman Bin Faisal University
A61K31/192A61K9/5115A61K9/5192B01J20/10B01J20/2808B01J20/28071B01J20/28073B01J20/28076B01J20/28083B01J20/3057B01J20/3078C01B37/005C01P2002/60C01P2006/10C01P2006/12C01P2006/14C01P2006/16
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Quick Facts
Patent No.
US 11,096,911
App. No.
16/138,591
Granted
Aug 24, 2021
Kind
B2
Abstract

A mesosilicalite nanocarrier having a hierarchical silicalite characterized by a molar ratio of aluminum to silica in a range of 1:3000 to 1:1000. The hierarchical silicalite includes mesopores of a hexagonal structure, and micropores of silicalite structure with a microporous volume in the range of 0.05 cc/g to 0.1 cc/g. The nanocarrier has a mesophase content in the range of 30 wt % to 70 wt %, a microphase content in the range of 30 wt % to 70 wt %, and a mean pore diameter in the range of 1.5 nm to 5.5 nm. A method of preparing the stable mesosilicalite nanocarrier with hierarchical micro/mesopores to load an antioxidant or drug for targeted drug delivery is also described.

Claims (31)

1. A method of preparing a mesosilicalite nanocarrier comprising:

a hierarchical silicalite having a silica to aluminum molar ratio in a range of 1000:1 to 3000:1, comprising:

a mesophase with mesopores of a hexagonal structure; and

a microphase with micropores of a microporous volume in the range of 0.05 cc/g to 0.1 cc/g;

wherein the mesophase content is in the range of 30% to 70% relative to a total weight of the nanocarrier, and the microphase content is in the range of 30% to 70% relative to the total weight of the nanocarrier; and

wherein a mean pore diameter of the mesosilicalite nanocarrier is in the range of 1.5 nm to 5.5 nm,

the method comprising:

mixing a silica source with a template to form a first mixture,

hydrothermally aging the first mixture at a temperature of 150° C.-200° C. for 24 hours to 86 hours to produce an aged first mixture;

drying the aged first mixture to form a silicalite;

treating the silicalite with an alkaline solution and a surfactant to form a second mixture;

hydrothermally aging the second mixture at a temperature of 60° C.-120° C. for 12 hours to 36 hours at a rate of 3° C./min to 6° C./min to form an aged second mixture;

neutralizing a pH of the aged second mixture;

hydrothermally aging the aged second mixture at a temperature of 60° C.-120° C. for 12 hours to 36 hours at a rate of 3° C./min to 6° C./min to produce a third mixture; and

drying the third mixture to form the mesosilicalite nanocarrier.

2. The method of claim 1 , wherein the silica source is colloidal silica.

3. The method of claim 2 , wherein the colloidal silica has a surface area in the range of 120 m 2 /g to 150 m 2 /g.

4. The method of claim 3 , wherein the colloidal silica has a density in the range of 1.15 g/mL to 1.35 g/mL at 20° C.-30° C.

5. The method of claim 1 , wherein the silicalite is a crystal having a crystal size of 1 μm to 5 μm.

6. The method of claim 1 , further comprising calcining the silicalite after the drying at a temperature in the range of 545° C.-605° C. for 5 hours to 11 hours and at a rate of 3° C./min to 6° C./min.

7. The method of claim 1 , further comprising calcining the mesosilicalite nanocarrier in a temperature range of 545° C.-605° C.

8. The method of claim 1 , wherein the template is tetrapropylammonium hydroxide.

9. The method of claim 1 , wherein the surfactant is at least one of an alkylammonium halide or an alkylammonium hydroxide.

10. The method of claim 9 , wherein the surfactant is cetyl trimethylammonium bromide.

11. The method of claim 1 , wherein the alkaline solution comprises a base selected from the group consisting of sodium hydroxide, potassium hydroxide, lithium hydroxide, and barium hydroxide in a concentration range of 0.1 M to 0.8 M.

12. The method of claim 1 , wherein the alkaline solution consists of sodium hydroxide in water at a concentration of 0.2 M to 0.7 M.

13. The method of claim 1 , further comprising loading the antioxidant into the mesosilicate nanocarrier, the loading comprising:

drying the mesosilicate nanocarrier at 100° C.-120° C. for 72 hours to 86 hours; and

mixing the dried mesosilicate nanocarrier with a solution of the antioxidant for 12 hours to 36 hours at 23° C.-30° C. to form the mesosilicate nanocarrier loaded with the antioxidant at 10% to 50% by weight of a total weight of the mesosilicate nanocarrier.

14. The method of claim 13 , wherein the solution of the antioxidant is an acidic aqueous solution.

15. The method of claim 13 , wherein the solution of the antioxidant has an antioxidant concentration of 0.25 g/L to 15 g/L.

Continuity (2)
Division 15478794 · Apr 4, 2017
Related Publication 20190022007A1 · Jan 24, 2019
Cited By (2)
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