Monolithic silicone and method of separation, purification and concentration therewith

Patent metadata

Field	Value
Publication number	US-9285300-B2
Application number	US-201213629723-A
Country	US
Kind code	B2
Filing date	Sep 28, 2012
Priority date	Sep 19, 2012
Publication date	Mar 15, 2016
Grant date	Mar 15, 2016

Abstract

The present invention provides a monolithic silicone in the form of an aerogel or a xerogel having flexibility and capable of dissolving molecules of a substance. This silicone monolithic body having continuous through passages is synthesized by copolymerizing starting materials of both a bifunctional alkoxysilane and a trifunctional alkoxysilane or tri- or higher functional alkoxysilanes through a sol-gel reaction for forming a Si—O network while causing phase separation.

First claim

What is claimed is:

1. A monolithic silicone, comprising a continuous silicone skeleton in the form of an aerogel or a xerogel containing continuous through pores,
the continuous silicone skeleton also comprising a copolymerized silane of both a bifunctional alkoxysilane and a trifunctional alkoxysilane or tri- or higher functional alkoxysilanes, forming a Si—O network,
wherein one or more of two functional groups of the bifunctional alkoxysilane, other than alkoxy groups, are selected from the group consisting of a phenyl group, a fluoroalkyl group, a vinyl group and a mercaptopropyl group.

2. The monolithic silicone according to claim 1 ,
wherein the continuous through pores have a pore diameter of 1 to 50 μm and the silicone skeleton has a diameter of 1 to 30 μm.

3. The monolithic silicone according to claim 2 ,
wherein the monolithic silicone exhibits flexibility between a temperature of liquid nitrogen to 320° C.

4. A method for producing a monolithic silicone comprising a step of:
copolymerizing silanes of both a bifunctional alkoxysilane and a trifunctional alkoxysilane or tri- or higher functional alkoxysilanes used as starting materials through a sol-gel reaction, whereby forming a Si—O network and causing phase separation,
producing an aerogel or a xerogel having continuous through pores and a silicone skeleton capable of absorbing chemical species,

wherein one or more of two functional groups of the bifunctional alkoxysilane, other than alkoxy groups, are selected from the group consisting of a phenyl group, a fluoroalkyl group, a vinyl group and a mercaptopropyl group.

5. The method for producing a monolithic silicone according to claim 4 ,
wherein the trifunctional alkoxysilane or higher functional alkoxysilanes has 6 functional groups and has a —Si—C—C—Si— or —Si-phenyl-Si— structure for forming the network of the monolithic silicone.

6. The method for producing a monolithic silicone according to claim 4 ,
wherein an acid-base two-stage reaction based on hydrolysis of an acetic acid catalyst and urea is performed with the phase separation controlled by a surface active agent.

7. A method for treating a sample, comprising a step of using a monolithic silicone according to claim 1 for a pretreatment of a sample for separation, purification, concentration or analysis.

8. A method for treating a sample, comprising a step of using a monolithic silicone according to claim 2 for a pretreatment of a sample for separation, purification, concentration or analysis.

9. A method for treating a sample according to claim 7 , additionally comprising a step of mechanically expressing the monolithic silicone, extruding an extraction solvent retained in the through pores of the monolithic silicone and recovering the extraction solvent.

10. The method for treating a sample according to claim 8 , additionally comprising a step of mechanically expressing the monolithic silicone,
extruding an extraction solvent retained in the through pores of the monolithic silicone, and recovering the extraction solvent.

11. The method for treating a sample according to claim 9 , comprising a step of recovering the analytes or the chemical species simultaneously with the extraction solvent by the monolithic silicone, when performing homogeneous liquid-liquid extraction for extracting analytes or specific chemical species by using a small amount of solvent for a large amount of aqueous sample.

12. The method for treating a sample according to claim 10 , comprising a step of recovering the analytes or the chemical species simultaneously with the extraction solvent by the monolithic silicone, when performing homogeneous liquid-liquid extraction for extracting analytes or specific chemical species by using a small amount of solvent for a large amount of aqueous sample.

13. The method for treating a sample according to claim 7 , comprising a step of recovering an emulsion of the solvent including the analytes or the specific chemical species by the monolithic silicone, when extracting analytes or specific chemical species from a large amount of an aqueous sample with a small amount of solvent insoluble in water.

14. The method for treating a sample according to claim 9 , comprising a step of recovering an emulsion of the solvent including the analytes or the specific chemical species by the monolithic silicone, when extracting analytes or specific chemical species from a large amount of an aqueous sample with a small amount of solvent insoluble in water.

15. The method for treating a sample according to claim 10 , comprising a step of recovering an emulsion of the solvent including the analytes or the specific chemical species by the monolithic silicone, when extracting analytes or specific chemical species from a large amount of an aqueous sample with a small amount of solvent insoluble in water.

16. An apparatus for treating a sample comprising a monolithic silicone having a continuous silicone skeleton in the form of an aerogel or a xerogel containing continuous through pores,
the continuous silicone skeleton comprising a copolymerized silane of both a bifunctional alkoxysilane and a trifunctional alkoxysilane or tri- or higher functional alkoxysilanes forming a Si—O network,
wherein at least two functional groups of the bifunctional alkoxysilane, other than an alkoxy groups, are selected from the group consisting of a phenyl group, a fluoroalkyl group, a vinyl group and a mercaptopropyl group,
for performing a method for treating a sample according to claim 7 by using the monolithic silicone.

17. An apparatus for treating a sample comprising a monolithic silicone according to claim 16 , wherein the monolithic silicone contains continuous through pores having a pore diameter of 1 to 50 μm and a silicone skeleton having a diameter of 1 to 30 μm.

18. An apparatus for treating a sample according to claim 16 , further comprising:
a syringe to be charged with the monolithic silicone including a solvent; and
a plunger that may be inserted into the syringe for expressing the solvent included in the monolithic silicone from the monolithic silicone.

19. The sample treater according to claim 17 , further comprising:
a syringe to be charged with the monolithic silicone including a solvent; and
a plunger that may be inserted into the syringe for expressing the solvent included in the monolithic silicone from the monolithic silicone.

20. The monolithic silicone according to claim 1 , wherein
the trifunctional alkoxysilane or higher functional alkoxysilanes has 6 functional groups and has a —Si—C—C—Si— or —Si-phenyl-Si— structure.

Assignees

• Nakanishi Kazuki
• Kanamori Kazuyoshi
• Hayase Gen
• Furuno Masahiro
• Takei Yoshiyuki
• Gl Sciences Inc
• Univ Kyoto

Inventors

• Nakanishi Kazuki
• Kanamori Kazuyoshi
• Hayase Gen
• Furuno Masahiro
• Takei Yoshiyuki

Classifications

• B01J20/28042

  Shaped bodies; Monolithic structures · CPC title

• B01J2220/86

  Sorbents applied to inner surfaces of columns or capillaries · CPC title

• B01J20/264 Primary

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

• B01J20/291

  Gel sorbents · CPC title

• B01J20/28085

  being more than 50 nm, i.e. macropores · CPC title