Sonication for improved particle size distribution of core-shell particles

Patent metadata

Field	Value
Publication number	US-9511575-B2
Application number	US-201414152375-A
Country	US
Kind code	B2
Filing date	Jan 10, 2014
Priority date	Nov 17, 2010
Publication date	Dec 6, 2016
Grant date	Dec 6, 2016

Abstract

In one or more embodiments, a porous composite particulate material includes a plurality of composite particles including an acid-base-resistant core particle at least partially surrounded by one or more layers of acid-base-resistant shell particles. The shell particles are adhered to the core particle by a polymeric material. The shell particles and/or core particles may be made from an acid-base-resistant material that is stable in harsh chemical conditions. During application of the polymeric material/shell particle bilayer, the core particles are sonicated to homogenize the particle size distribution and minimize agglomeration of particles. Multiple bilayers of polymer/shell particles may be applied. In one embodiment, the core particle comprises generally spherical glassy carbon, while the shell particles may comprise nano-sized diamond particles. Other acid-base-resistant materials may be employed. The porous composite particulate materials may be used in separation technologies, including, but not limited to, chromatography and solid phase extraction.

First claim

What is claimed is:

1. A method for manufacturing a porous composite particulate material, comprising:
providing a plurality of acid-base-resistant core particles, wherein the plurality of acid-base-resistant core particles include carbon core particles;
providing a plurality of acid-base-resistant shell particles, wherein the plurality of acid-base-resistant shell particles include at least one of graphitic carbon shell particles or diamond shell particles;
applying sonic energy to the plurality of acid-base-resistant core particles; and
after the act of applying sonic energy, applying at least one polymer material/shell particle bilayer including:
coating at least a portion of the plurality of acid-base-resistant core particles, at least a portion of the plurality of acid-base-resistant shell particles, or combinations thereof with at least one polymer material; and
adhering a portion of the plurality of acid-base-resistant shell particles to at least some of the plurality of acid-base-resistant core particles with the at least one polymer material to form a plurality of composite particles.

2. The method of claim 1 wherein applying at least one polymer material/shell particle bilayer includes forming a plurality of polymer material/shell particle bilayers in separate layer-by-layer steps.

3. The method of claim 2 wherein from 5 to 100 of the plurality of polymer material/shell particle bilayers are formed.

4. The method of claim 2 wherein from 10 to 50 of the plurality of polymer material/shell particle bilayers are formed.

5. The method of claim 1 wherein the carbon core particles includes at least one of graphitic carbon or glassy carbon.

6. The method of claim 1 wherein the carbon core particles are generally spherical.

7. The method of claim 1 wherein the plurality of composite particles exhibits a particle size of at least about 0.5 μm and a surface area of at least about 5.0 m 2 /g.

8. The method of claim 1 wherein the plurality of acid-base-resistant core particles exhibits a particle size of at least an order of magnitude larger than the plurality of acid-base-resistant shell particles.

9. The method of claim 1 wherein the at least one polymer material is coated on the core particles before adhering the shell particles to the core particles.

10. The method of claim 1 wherein the at least one polymer material is coated on the plurality of acid-base-resistant shell particles before adhering the plurality of acid-base-resistant shell particles to the plurality of acid-base-resistant core particles.

11. The method of claim 1 , further comprising applying sonic energy to the plurality of acid-base-resistant core particles during application of the at least one polymer material/shell particle bilayer.

12. The method of claim 11 wherein applying sonic energy to the plurality of acid-base-resistant core particles during application of the at least one polymer material/shell particle bilayer includes applying sonic energy after coating the at least one polymer material on the plurality of acid-base-resistant core particles and prior to adhering the plurality of acid-base-resistant shell particles of any given bilayer.

13. The method of claim 11 wherein applying sonic energy to the plurality of acid-base-resistant core particles during application of the at least one polymer material/shell particle bilayer includes applying sonic energy during application of each bilayer.

14. The method of claim 1 wherein applying sonic energy to the plurality of acid-base-resistant core particles during application of the at least one polymer material/shell particle bilayer includes applying sonic energy during application of any given bilayer in a plurality of discontinuous intervals.

15. The method of claim 14 wherein a total sonication time associated with application of any given bilayer is about 1 minute to about 20 minutes, and wherein each interval is about 5% to about 50% of the total sonication time.

16. The method of claim 14 wherein a total sonication time associated with application of any given bilayer is about 2 minutes to about 10 minutes, and wherein each interval is about 10% to about 30% of the total sonication time.

17. The method of claim 1 , wherein the at least one polymeric material includes at least one amine polymer.

18. The method of claim 1 , further comprising at least partially cross-linking the at least one polymeric material.

19. A method for manufacturing a porous composite particulate material, comprising:
providing a plurality of acid-base-resistant generally spherical carbon core particles;
providing a plurality of acid-base-resistant shell particles, wherein the plurality of acid-base-resistant shell particles include graphitic carbon shell particles;
applying sonic energy to the plurality of acid-base-resistant generally spherical carbon core particles; and
after the act of applying sonic energy, applying at least one polymer material/shell particle bilayer including:
coating at least a portion of the plurality of acid-base-resistant generally spherical carbon core, at least a portion of the plurality of acid-base-resistant shell particles, or combinations thereof with at least one amine polymer material; and
adhering a portion of the plurality of acid-base-resistant shell particles to at least some of the plurality of acid-base-resistant generally spherical carbon core with the at least one amine polymer material.

20. A method for manufacturing a porous composite particulate material, comprising:
providing a plurality of acid-base-resistant generally spherical carbon core particles;
providing a plurality of acid-base-resistant shell particles, wherein the plurality of acid-base-resistant shell particles include graphitic carbon shell particles;
applying sonic energy to the plurality of acid-base-resistant generally spherical carbon core particles; and
after the act of applying sonic energy,
coating at least a portion of the plurality of acid-base-resistant generally spherical carbon core with at least one amine polymer material; and
adhering a portion of the plurality of acid-base-resistant shell particles to the plurality of acid-base-resistant generally spherical carbon cores with the at least one amine polymer material.

Assignees

• Univ Brigham Young

Inventors

• Linford Matthew R
• Hung Chuan-Hsi

Classifications

• B01J20/28004 Primary

  Sorbent size or size distribution, e.g. particle size · CPC title

• B01J20/3289

  Coatings involving more than one layer of same or different nature · CPC title

• B01J20/3293

  Coatings on a core, the core being particle or fiber shaped, e.g. encapsulated particles, coated fibers · CPC title

• B32B38/0008 Primary

  Electrical discharge treatment, e.g. corona, plasma treatment; wave energy or particle radiation (heat treatment B32B38/0036) · CPC title

• B01J20/286

  Phases chemically bonded to a substrate, e.g. to silica or to polymers · CPC title