IP Library Granted Patent US 11,964,252
Granted Patent B2
US 11,964,252 · App. 17/157,526 · Granted Apr 23, 2024

Sorbent and devices for capturing, stabilizing, and recovering volatile and semi-volatile compounds

Inventors: Shoaib F. Shaikh (Stillwater, OK); Allen W. Apblett (Stillwater, OK); Nicholas F. Materer (Stillwater, OK); Evgueni Kadossov (Stillwater, OK); Michael L. Teicheira (Stillwater, OK)
Assignee: XPLOSAFE, LLC
B01J20/103B01D53/02B01J20/28021B01J20/28064B01J20/28073B01J20/28076B01J20/28083B01J20/3204B01J20/3219B01J20/3246B01J20/3293C01B33/18C06B21/0091C06B23/00C06B45/00F42D5/04B01D2253/106B01D2257/708B01D2259/4583C01P2002/82C01P2004/04C01P2004/13C01P2006/12C01P2006/14C01P2006/16
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Quick Facts
Patent No.
US 11,964,252
App. No.
17/157,526
Granted
Apr 23, 2024
Kind
B2
Abstract

The present invention provides an improved sorbent and corresponding device(s) and uses thereof for the capture and stabilization of volatile organic compounds (VOC) or semi-volatile organic compounds (SVOC) from a gaseous atmosphere. The sorbent is capable of rapid and high uptake of one or more compounds and provides quantitative release (recovery) of the compound(s) when exposed to elevated temperature and/or organic solvent. Uses of particular improved grades of mesoporous silica are disclosed.

Claims (60)

1. A flexible device for passive sampling of volatile organic compound or semi-volatile organic compound in air or gaseous environment, the device comprising

a flexible facing layer;

a flexible intermediate layer;

a flexible backing layer comprising attachment means; and

one or more sorbent-holding containers disposed between said facing layer and said intermediate layer, said containers retaining respective charges of sorbent; wherein

said facing layer, said intermediate layer, and said one or more sorbent-holding containers are permeable to volatile organic compound (VOC) and/or semi-volatile organic compound (SVOC).

2. The device of claim 1 , wherein a) said facing layer and said intermediate layer are independently selected upon each occurrence from a mesh, fabric, foam, material through which VOC or SVOC can pass, or any combination thereof; b) said device further comprises one or more non-permeable sorb ent-holding containers comprising VOC- and SVOC-impermeable material defining a sealed chamber retaining a charge of sorbent; c) said device further comprises VOC- and SVOC-impermeable packaging material enclosing said device; d) said one or more porous sorbent-holding containers is replaceable; e) said device is reusable; f) said device further comprises VOC- and SVOC-impermeable packaging material enclosing said one or more sorbent-holding containers; g) said backing layer is non-permeable to VOC or SVOC; h) said backing layer is permeable to VOC or SVOC; i) one or more of said one or more sorbent-holding containers (along with its respective charge of sorbent) is replaced with a compressed article or loose powder comprising said sorbent; or j) a combination of any two or more of the above.

3. The device of claim 2 , wherein a) said one or more sorbent-holding containers is flexible; b) said one or more sorbent-holding containers is independently selected upon each occurrence from the group consisting of cartridge, tube, wafer, pouch, sphere, or rod; c) said one or more sorbent-holding containers comprises PTFE (polytetrafluoroethylene); d) said intermediate layer comprises PTFE; e) said mesh comprises PTFE, polypropylene, PTFE-coated wire, and/or other material adapted for making a breathable mesh; f) said attachment means comprises hook-and-loop attachment, adhesive, or magnet; or g) a combination of any two or more of the above.

4. The device of claim 2 , wherein said respective charges of sorbent are independently selected upon each occurrence from one or more portions of mesoporous silica sorbent of the MCM-41 type (hexagonal), wherein the mesoporous silica possesses a combination of two or more of the following physical properties:

Property

Linear formula

SiO 2 polymer

Pore structure

Hexagonal tubes

Pore size (diameter)

about 2 to about 30 nm

Pore volume

about 0.5 to about 2.0 cm 3 /g

Surface area

greater than about 600 m 2 /g

Channel wall thickness

about 1 to about 5 nm

5. The device of claim 4 , wherein the mesoporous silica comprises: a) at least one non-functionalized mesoporous silica; b) at least one functionalized mesoporous silica; c) said sorbent excludes a porous polymer; d) a combination of one or more non-functionalized mesoporous silica and one or more functionalized mesoporous silica; e) the sorbent in said one or more sorbent-holding containers is the same as the sorbent in said one or more non-permeable sorbent-holding containers; or f) a combination of any two or more of the above.

6. The device of claim 5 , wherein the weight ratio of non-functionalized mesoporous silica to functionalized mesoporous silica range from about 1:100 to about 100:1.

7. The device of claim 4 , wherein the sorbent has been functionalized with one or more adsorption modifier functional groups that improve in at least one aspect the adsorption of particular VOC or SVOC.

8. The device of claim 7 , wherein: a) the one or more adsorption modifier functional groups are covalently bound to the porous medium; b) the one or more adsorption modifier functional groups are non-covalently bound to the porous medium; c) the mass content of functional groups in the porous medium as determined by thermogravimetric analysis is in the range of 20-25%; or d) a combination of any two or more thereof.

9. The device of claim 5 , wherein the sorbent is silane-functionalized mesoporous silica.

10. The device according to claim 9 , wherein the silane functionalized mesoporous silica has been functionalized by treating unfunctionalized mesoporous silica with a trialkoxyalkylsilane (R 1 Si(OR 2 ) 3 ), wherein:

R 1 is selected from the group consisting of aromatic group, alkyl group, oxygen-containing alkyl groups, sulfur-containing alkyl groups, nitrogen-containing alkyl groups, phenyl, biphenyl, (C1-C8)-alkyl, methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decanyl, undecanyl, methoxytriethyleneoxypropyl, alkoxyalkyleneoxyalkyl, haloalkyl, halo-(C1-C8)-alkyl, aminoalkyl, alkoxyalkyl, polyaromatic, toluyl, fluoroalkyls, fluroaromatics, and their combinations; and

R 2 is selected from the group consisting of alkyl, C1-C12-alkyl, with methyl, ethyl, and propyl being preferred, thereby forming a silane-functionalized mesoporous silica comprising plural silane groups R 1 Si-covalently bound to oxygen molecules of the mesoporous silica.

11. The device of claim 9 , wherein the silane functionalized mesoporous silica comprises functional groups with a chemical formula defined as —Si(R 1 )(OR 2 ) n —O m —, wherein:

R 1 is selected from the group consisting of aromatic group, alkyl group, oxygen-containing alkyl group, phenyl, biphenyl, C1-C8-alkyl, methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decanyl, undecanyl, methoxytriethyleneoxypropyl, alkoxyalkyleneoxyalkyl, haloalkyl, alkoxyalkyl, polyaromatic, and toluyl;

R 2 is selected from the group consisting of alkyl, C1-C12-alkyl, methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decanyl, and undecanyl,

thereby forming a silane-functionalized mesoporous silica comprising plural silane groups R 1 Si-covalently bound to oxygen molecules of the mesoporous silica; and

wherein n is 0, 1 or 2, and m is 2, 1, or 0, respectively.

12. The device of claim 1 , wherein a) the sorbent releases at least 75 wt % of adsorbed VOC or SVOC when the sorbent is exposed to heat or organic solvent; and/or b) the sorbent releases less than 25% of VOC or SVOC during storage at ambient temperature for a period of at least 1 week.

13. A flexible device for passive sampling of volatile organic compound or semi-volatile organic compound in air or gaseous environment, the device comprising

a flexible facing layer;

a flexible intermediate layer;

a flexible backing layer comprising attachment means; and

one or more sorbent-holding containers disposed between said facing layer and said intermediate layer, said containers retaining respective charges of sorbent;

one or more non-permeable sorbent-holding containers comprising VOC- and SVOC-impermeable material defining a sealed chamber retaining a charge of sorbent; wherein

said facing layer, said intermediate layer, and said one or more sorbent-holding containers are permeable to volatile organic compound (VOC) and/or semi-volatile organic compound (SVOC).

14. The device of claim 13 , wherein a) said facing layer and said intermediate layer are independently selected upon each occurrence from a mesh, fabric, foam, material through which VOC or SVOC can pass, or any combination thereof; b) said device further comprises VOC- and SVOC-impermeable packaging material enclosing said device; c) said one or more porous sorbent-holding containers is replaceable; d) said device is reusable; e) said device further comprises VOC- and SVOC-impermeable packaging material enclosing said one or more sorbent-holding containers; f) said backing layer is non-permeable to VOC or SVOC; g) said backing layer is permeable to VOC or SVOC; h) one or more of said one or more sorbent-holding containers (along with its respective charge of sorbent) is replaced with a compressed article or loose powder comprising said sorbent; or i) a combination of any two or more of the above.

15. The device of claim 14 , wherein a) said one or more sorbent-holding containers is flexible; b) said one or more sorbent-holding containers is independently selected upon each occurrence from the group consisting of cartridge, tube, wafer, pouch, sphere, or rod; c) said one or more sorbent-holding containers comprises PTFE (polytetrafluoroethylene); d) said intermediate layer comprises PTFE; e) said mesh comprises PTFE, polypropylene, PTFE-coated wire, and/or other material adapted for making a breathable mesh; f) said attachment means comprises hook-and-loop attachment, adhesive, or magnet; or g) a combination of any two or more of the above.

16. The device of claim 14 , wherein said respective charges of sorbent are independently selected upon each occurrence from one or more portions of mesoporous silica sorbent of the MCM-41 type (hexagonal), wherein the mesoporous silica possesses a combination of two or more of the following physical properties:

Property

Linear formula

SiO 2 polymer

Pore structure

Hexagonal tubes

Pore size (diameter)

about 2 to about 30 nm

Pore volume

about 0.5 to about 2.0 cm 3 /g

Surface area

greater than about 600 m 2 /g

Channel wall thickness

about 1 to about 5 nm

17. The device of claim 16 , wherein the mesoporous silica comprises: a) at least one non-functionalized mesoporous silica; b) at least one functionalized mesoporous silica; c) said sorbent excludes a porous polymer; d) a combination of one or more non-functionalized mesoporous silica and one or more functionalized mesoporous silica; e) the sorbent in said one or more sorbent-holding containers is the same as the sorbent in said one or more non-permeable sorbent-holding containers; or f) a combination of any two or more of the above.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 2, 2021
From: SHAIKH, SHOAIB F.; APBLETT, ALLEN W.; MATERER, NICHOLAS F.; KADOSSOV, EVGUENI; TEICHEIRA, MICHAEL L.
To: XPLOSAFE, LLC
Reel/Frame 055460/0260 →
Continuity (8)
Continuation In Part 17116492 · Dec 9, 2020
Continuation In Part PCTUS2019043140 · Jul 24, 2019
Continuation PCTUS2019043140 · Jul 24, 2019
Continuation 16224049 · Dec 18, 2018
Continuation In Part 16045435 · Jul 25, 2018
Continuation In Part 15137055 · Apr 25, 2016
Provisional Application 62152439 · Apr 24, 2015
Related Publication 20210260562A1 · Aug 26, 2021