Aerogel precursor and aerogel prepared using the same

Patent metadata

Field	Value
Publication number	US-11078084-B2
Application number	US-201615736725-A
Country	US
Kind code	B2
Filing date	Dec 15, 2016
Priority date	Mar 16, 2016
Publication date	Aug 3, 2021
Grant date	Aug 3, 2021

Abstract

The present disclosure provides an aerogel precursor including an alkoxydisiloxane-based prepolymer and having a functional group derived from a hydrophobic sol-gel forming agent of the following Chemical Formula 1 on a surface thereof, and therefore, capable of enhancing high temperature thermal stability of an aerogel providing hydrophobic pores having uniform pore size distribution when preparing an aerogel, and an aerogel prepared using the same:(in Chemical Formula 1, M, R, R1 to R4 are the same as defined in the specification.)

First claim

What is claimed is:

1. An aerogel precursor comprising an alkoxydisiloxane-based prepolymer, and having a functional group derived from a hydrophobic sol-gel forming agent of the following Chemical Formula 2 on a surface thereof:

wherein:
M 11 is any one selected from the group consisting of group 4 elements and group 14 elements;
R 11 is a halogen group;
R 12 and R 13 each independently is selected from the group consisting of an alkyl group having 1 to 20 carbon atoms, an alkenyl group having 2 to 20 carbon atoms, an alkynyl group having 2 to 20 carbon atoms, a cycloalkyl group having 3 to 20 carbon atoms, an aryl group having 6 to 20 carbon atoms, an arylalkyl group having 7 to 20 carbon atoms and an alkylaryl group having 7 to 20 carbon atoms; and
R 14 is selected from the group consisting of an alkyl group having 2 to 20 carbon atoms, an alkenyl group having 2 to 20 carbon atoms, an alkynyl group having 2 to 20 carbon atoms, a cycloalkyl group having 3 to 20 carbon atoms, an aryl group having 6 to 20 carbon atoms, an arylalkyl group having 7 to 20 carbon atoms and an alkylaryl group having 7 to 20 carbon atoms,
wherein the alkoxydisiloxane-based prepolymer has a degree of hydrolysis of 50% to 85%, and
the alkoxydisiloxane-based prepolymer includes an alkoxydisiloxane-derived repeating unit having a molecular weight of 60 Da to 140 Da and a molecular weight distribution with an m/z (ratio of mass to charge) value of 620 to 1,800 when analyzing the mass by MALDI-TOF.

2. The aerogel precursor of claim 1 , wherein M is selected from the group consisting of Ti, Hf, Si and Zr.

3. The aerogel precursor of claim 1 , wherein:
M 11 is Si;
R 11 is a chloro group, a bromo group or an iodo group; and
R 12 and R 13 each independently is selected from the group consisting of an alkyl group having 1 to 12 carbon atoms, an aryl group having 6 to 12 carbon atoms, an arylalkyl group having 7 to 13 carbon atoms and an alkylaryl group having 7 to 13 carbon atoms; and
R 14 is selected from the group consisting of an alkyl group having 2 to 12 carbon atoms, an aryl group having 6 to 12 carbon atoms, an arylalkyl group having 7 to 13 carbon atoms and an alkylaryl group having 7 to 13 carbon atoms.

4. The aerogel precursor of claim 3 , wherein, in Chemical Formula 2:
R 11 is a chloro group or a bromo group;
R 12 and R 13 each independently is selected from the group consisting of an alkyl group having 1 to 12 carbon atoms, an aryl group having 6 to 12 carbon atoms, an arylalkyl group having 7 to 13 carbon atoms and an alkylaryl group having 7 to 13 carbon atoms; and
R 14 is selected from the group consisting of an alkyl group having 2 to 12 carbon atoms, an aryl group having 6 to 12 carbon atoms, an arylalkyl group having 7 to 13 carbon atoms and an alkylaryl group having 7 to 13 carbon atoms.

5. The aerogel precursor of claim 1 , wherein the hydrophobic sol-gel forming agent includes any one or a mixture of two or more selected from the group consisting of chlorotriethylsilane, bromotriethylsilane and chloro(methyl)diphenylsilane.

6. The aerogel precursor of claim 1 , wherein the functional group derived from the hydrophobic sol-gel forming agent is included in 0.1 mol % to 60 mol % with respect to a total mole of the alkoxy group in the alkoxydisiloxane-based prepolymer.

7. The aerogel precursor of claim 1 , which has a carbon content of 20% by weight or greater with respect to a total weight of the aerogel precursor.

8. A method for preparing the aerogel precursor of claim 1 , the method comprising:
preparing the alkoxydisiloxane-based prepolymer having a molecular weight distribution with an m/z (ratio of mass to charge) value of 620 to 3,000 when analyzing the mass by MALDI-TOF by hydrolyzing and polycondensation reacting an alkoxysilane-based compound; and
reacting the alkoxydisiloxane-based prepolymer with the hydrophobic sol-gel forming agent of Chemical Formula 2:

wherein:
M 11 is any one selected from the group consisting of group 4 elements and group 14 elements;
R 11 is a halogen group;
R 12 and R 13 each independently is selected from the group consisting of an alkyl group having 1 to 20 carbon atoms, an alkenyl group having 2 to 20 carbon atoms, an alkynyl group having 2 to 20 carbon atoms, a cycloalkyl group having 3 to 20 carbon atoms, an aryl group having 6 to 20 carbon atoms, an arylalkyl group having 7 to 20 carbon atoms and an alkylaryl group having 7 to 20 carbon atoms; and
R 14 is selected from the group consisting of an alkyl group having 2 to 20 carbon atoms, an alkenyl group having 2 to 20 carbon atoms, an alkynyl group having 2 to 20 carbon atoms, a cycloalkyl group having 3 to 20 carbon atoms, an aryl group having 6 to 20 carbon atoms, an arylalkyl group having 7 to 20 carbon atoms and an alkylaryl group having 7 to 20 carbon atoms.

9. The method for preparing the aerogel precursor of claim 8 , wherein the alkoxysilane-based compound includes tetraethoxysilane.

10. The aerogel precursor of claim 1 , wherein M 11 is Si.

11. An aerogel precursor comprising an alkoxydisiloxane-based prepolymer, and having a functional group derived from a hydrophobic sol-gel forming agent of the following Chemical Formula 3 on a surface thereof, wherein the hydrophobic sol-gel forming agent includes a compound of the following Chemical Formula 3:

wherein, in Chemical Formula 3,
M 21 is Ti or Zr; and
R 21 to R 24 are each independently a hydrophobic functional group selected from the group consisting of an alkyl group having 1 to 10 carbon atoms, a cycloalkyl group having 3 to 12 carbon atoms, an aryl group having 6 to 12 carbon atoms, an arylalkyl group having 7 to 13 carbon atoms, an alkylaryl group having 7 to 13 carbon atoms; or a functional group reactive with the alkoxydisiloxane-based prepolymer that is a halogen group or an alkoxy group having 1 to 10 carbon atoms, however, R 21 to R 24 are not a hydrophobic functional group or a functional group reactive with the alkoxydisiloxane-based prepolymer at the same time,
wherein the alkoxydisiloxane-based prepolymer has a degree of hydrolysis of 50% to 85%, and
the alkoxydisiloxane-based prepolymer includes an alkoxydisiloxane-derived repeating unit having a molecular weight of 60 Da to 140 Da and a molecular weight distribution with an m/z (ratio of mass to charge) value of 620 to 1,800 when analyzing the mass by MALDI-TOF.

12. The aerogel precursor of claim 11 , wherein, in Chemical Formula 3, M 12 is Ti.

13. An aerogel precursor comprising an alkoxydisiloxane-based prepolymer, and having a functional group derived from a hydrophobic sol-gel forming agent of the following Chemical Formula 2 on a surface thereof:

wherein:
M 11 is any one selected from the group consisting of group 4 elements and group 14 elements;
R 11 is a halogen group;
R 12 and R 13 each independently is selected from the group consisting of an alkyl group having 1 to 20 carbon atoms, an alkenyl group having 2 to 20 carbon atoms, an alkynyl group having 2 to 20 carbon atoms, a cycloalkyl group having 3 to 20 carbon atoms, an aryl group having 6 to 20 carbon atoms, an arylalkyl group having 7 to 20 carbon atoms and an alkylary

Assignees

• Lg Chemical Ltd

Inventors

• Choi Hee Jung
• Oh Kyoung Shil
• Chang Yeong Rae
• Lee Je Kyun

Classifications

• C01B33/158

  Purification; Drying; Dehydrating · CPC title

• B01J13/0091

  Preparation of aerogels, e.g. xerogels · CPC title

• C07F7/08

  Compounds having one or more C—Si linkages · CPC title

• C09K3/30

  for aerosols (aerosol containers B65D83/14) · CPC title

• C07F7/0874

  Reactions involving a bond of the Si-O-Si linkage · CPC title