MONOLITHIC SILICONE AND METHOD OF SEPARATION, PURIFICATION AND CONCENTRATION THEREWITH

• US 20140076070A1
• Filed: 09/28/2012
• Published: 03/20/2014
• Est. Priority Date: 09/19/2012
• Status: Active Grant

• Current Assignee: GL Sciences Incorporated, Kyoto University
• Original Assignee: GL Sciences Incorporated
• Inventors: Nakanishi, Kazuki, Kanamori, Kazuyoshi, Furuno, Masahiro, Hayase, Gen, Takei, Yoshiyuki
• Granted Patent: US 9,285,300 B2
• Time in Patent Office: Days
• US Class Current: 73/863.23
• CPC Class Codes: B01J 20/264 derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
• CPC Class Codes: B01J 20/28042 Shaped bodies; Monolithic structures
• CPC Class Codes: B01J 20/28047 Gels
• CPC Class Codes: B01J 20/28085 being more than 50 nm, i.e. macropores
• CPC Class Codes: B01J 20/291 Gel sorbents
• CPC Class Codes: B01J 2220/86 Sorbents applied to inner surfaces of columns or capillaries
• CPC Class Codes: G01N 1/28 Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Qmounting specimens on microscopic slides G02B21/34; means for supporting the objects or the materials to be analysed in electron microscopes H01J37/20 ; laboratory gas handling apparatus B01L5/00
• CPC Class Codes: G01N 2001/4061 Solvent extraction

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.

Claims

1. A monolithic silicone, comprising a continuous silicone skeleton in the form of an aerogel or a xerogel to create through pores of a predetermined size.

2. The monolithic silicone according to claim 1,

wherein the continuous through pores have a pore diameter of 1 to 50 μ

m and the silicone skeleton has a diameter of 1 to 30 μ

m.

4. The monolithic silicone according to claim 2,

wherein the monolithic silicone exhibits flexibility between a temperature of liquid nitrogen to 320°

C.

10. 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.

11. 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.

12. A method for treating a sample according to claim 10, 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.

13. The method for treating a sample according to claim 11, 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.

16. The method for treating a sample according to claim 12, 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.

17. The method for treating a sample according to claim 13, 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.

18. 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.

20. The method for treating a sample according to claim 12, 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.

21. The method for treating a sample according to claim 13, 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.

22. An apparatus for treating a sample comprising a monolithic silicone having a silicone skeleton in the form of an aerogel or a xerogel and a Si—

O network bound to the silicone skeleton to create through pores of a predetermined size, wherein the through pores contact the silicone skeleton, for performing a method for treating a sample according to claim 10 by using the monolithic silicone.

24. An apparatus for treating a sample comprising a monolithic silicone according to claim 22, wherein the monolithic silicon contains continuous through pores having a pore diameter of 1 to 50 μ

m and a silicone skeleton having a diameter of 1 to 30 μ

m.

26. An apparatus for treating a sample according to claim 22, 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.

28. The sample treater according to claim 24, 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.

3. (canceled)

5. 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.

6. The method for producing a monolithic silicone according to claim 5,

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

7. The method for producing a monolithic silicone according to claim 5,

wherein the starting materials include, as a crosslinking agent, an alkoxysilane having a —

Si—

C—

C—

Si—

or —

Si-phenyl-Si—

structure for forming the network of the monolithic silicone.

9. The method for producing a monolithic silicone according to claim 5,

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.

8. (canceled)

14-15. -15. (canceled)

19. (canceled)

23. (canceled)

25. (canceled)

27. (canceled)

29. (canceled)