Superpolar chromatographic stationary phases and extraction sorbents and their methods of synthesis

Patent metadata

Field	Value
Publication number	US-9700872-B1
Application number	US-201615200224-A
Country	US
Kind code	B1
Filing date	Jul 1, 2016
Priority date	Jul 1, 2016
Publication date	Jul 11, 2017
Grant date	Jul 11, 2017

Abstract

A superpolar sorbent network is a sol-gel network of at least one metal oxide precursor condensed and at least one polyhydroxy molecule. The metal oxide precursor is a silicate precursor, aluminate precursor, titanate precursor, zirconate precursor, germinate precursor, or any combinations thereof, and the polyhydroxy molecule has a multiplicity of hydroxyl groups. The polyhydroxy molecule can be an organic molecule derived from nature. The superpolar sorbent network can be used as a particulate or bulk sorbent for sampling or removal of analytes or contaminants from an environment or can be coated on a tube or particulate substrate for use as a chromatographic stationary phase.

First claim

We claim:

1. A superpolar sorbent network, comprising a sol-gel network of at least one metal oxide precursor condensed with at least one polyhydroxy molecule where the network comprises units with metal-oxygen-metal groups and units with metal-oxygen-carbon groups respectively bonded to the at least one polyhydroxy molecule of one or more of the structures:

where there is a random placement of units within the network, where units from tetraalkoxysilanes are 0-100 weight percent of the network, where units from trialkoxysilanes are 0 to 100 weight percent of the network, and optionally comprising units from dialkoxysilanes at 0 to 99 weight percent of the network, where the polyhydroxy molecule has differing patterns and degrees of condensation, where optionally, the silicon-oxygen-silicon groups and the silicon-oxygen-carbons groups of the structure are replaced with metal-oxygen-metal groups and metal-oxygen-carbon groups of another metal where the another metal is aluminum, titanium, zirconium, or germanium from at least one aluminate precursor, titanate precursor, zirconate precursor, or germinate precursor, and where, optionally, the polyhydroxy units from sucrose are replaced with the polyhydroxy units of an another organic molecule comprising a multiplicity of hydroxyl groups.

2. The superpolar sorbent network according to claim 1 , wherein the metal oxide precursor is a tetraalkoxysilane, trialkoxysilane, or a combination of at least one of the tetraalkoxysilane and trialkoxysilane with a dialkoxysilane.

3. The superpolar sorbent network according to claim 1 , wherein the another organic molecule is Sucrose-6-phosphate, Sucrose6F-phosphate, 2-Cyanoethylsucrose, Sucralose, 1-Ketose, UDP-alpha-D-glucose, Uridine Diphosphate Glucose, Sorbitol, or any mixture thereof.

4. The superpolar sorbent network according to claim 1 , wherein the metal oxide precursor is tetramethoxysilane and the polyhydroxy molecule comprises sucrose.

5. The superpolar sorbent network according to claim 1 , wherein the metal oxide precursor is methyltrimethoxysilane and the polyhydroxy molecule comprises sucrose.

6. The superpolar sorbent network according to claim 1 , wherein the at least one metal oxide precursor includes an unsubstituted or substituted arytrialkoxysilane.

7. The superpolar sorbent network according to claim 1 , wherein the at least one metal oxide precursor includes an unsubstituted or substituted alkyltrialkoxysilane.

8. A sampling device or analytical device comprising a superpolar sorbent network according to claim 1 , wherein the sampling device is an extraction device or a chromatography device.

9. The sampling device or analytical device according to claim 8 , wherein the extraction device is a fiber superpolar microextraction fiber, superpolar microextraction tube, superpolar microextraction membrane, superpolar microextraction stir bar, superpolar microextraction fabric, superpolar microextraction capsule, or superpolar microextraction vial.

10. The sampling device or analytical device according to claim 8 , wherein the extraction device is a solid phase extractor selected from a matrix solid phase dispersant, a magnetic solid phase extractor, or a dynamic fabric phase sorptive extractor.

11. The sampling device or analytical device according to claim 8 , wherein the analytical device is a gas chromatograph or a liquid chromatograph.

12. A method of preparing a superpolar sorbent network according to claim 1 , comprising:
providing at least one metal oxide precursor;
providing at least one polyhydroxy molecule;
providing water;
providing a catalyst;
optionally, providing a solvent;
combining the at least one metal oxide precursor, the at least one polyhydroxy molecule, the water, the catalyst, and, optionally, the solvent to form a sol;
hydrolyzing the sol, wherein the at least one metal oxide precursors form hydrolyzed metal oxide precursors; and
condensing the hydrolyzed metal oxide precursors and the at least one polyhydroxy molecules to form a gel that provides the superpolar sorbent network.

13. The method according to claim 12 , wherein condensing occurs with heating of the sol.

14. The method according to claim 12 , further comprising coating the sol on a substrate, wherein the superpolar sorbent network comprises a coating on the substrate.

15. The method according to claim 14 , wherein the substrate is a metal oxide particle, a metal tube, a silica fiber, a fabric, a glass tube, a glass sheet, or a vial.

Assignees

• Kabir Abuzar
• Furton Kenneth G
• Univ Florida Int

Inventors

• Kabir Abuzar
• Furton Kenneth G

Classifications

• B01J20/28042

  Shaped bodies; Monolithic structures · CPC title

• B01J20/264

  derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers · CPC title

• B01D15/22 Primary

  relating to the construction of the column · CPC title

• B01J20/288 Primary

  Polar phases · CPC title

• B01J20/285

  based on polymers · CPC title