Method for producing aerogel blanket and aerogel blanket produced thereby

Patent metadata

Field	Value
Publication number	US-11274044-B2
Application number	US-201715569056-A
Country	US
Kind code	B2
Filing date	Mar 8, 2017
Priority date	Mar 8, 2016
Publication date	Mar 15, 2022
Grant date	Mar 15, 2022

Abstract

The present invention relates to a method for producing an aerogel blanket exhibiting excellent hydrophobicity at high temperatures and an aerogel blanket produced thereby. The present invention uses a mixture of silica sol and a hydrophobic aerogel powder as an aerogel precursor and thus can achieve hydrophobicity in the internal structure as well as on the surface of the aerogel included in the aerogel blanket. Accordingly, the aerogel blanket can attain high hydrophobicity and thus can exhibit excellent hydrophobicity retention ability even in high-temperature applications.

First claim

The invention claimed is:

1. A method of producing an aerogel blanket, the method comprising:
1) mixing a hydrophobic aerogel powder with silica sol to produce an aerogel precursor;
2) after producing the aerogel precursor, producing a wet gel-substrate composite by: (i) adding a basic catalyst to the aerogel precursor, (ii) depositing a mixture of the basic catalyst and the aerogel precursor onto a blanket substrate, and (iii) gelating the mixture;
3) after producing the wet gel-substrate composite, producing a hydrophobic wet gel-substrate composite by performing surface modification of the wet gel-substrate composite; and
4) after producing the hydrophobic wet gel-substrate composite, drying the hydrophobic wet gel-substrate composite.

2. The method of producing an aerogel blanket according to claim 1 , wherein the hydrophobic aerogel powder is a silica aerogel powder.

3. The method of producing an aerogel blanket according to claim 1 , wherein the hydrophobic aerogel powder is a hydrophobic aerogel powder having a carbon content of 10 to 12 parts by weight with respect to a total weight of the aerogel powder.

4. The method of producing an aerogel blanket according to claim 1 , wherein the hydrophobic aerogel powder is used in an amount of 25 parts to 50 parts by weight with respect to 100 parts by weight of silica contained in the silica sol.

5. The method of producing an aerogel blanket according to claim 1 , wherein the hydrophobic aerogel powder is an organic functional aerogel powder.

6. The method of producing an aerogel blanket according to claim 5 , wherein the organic functional aerogel powder is produced by reacting silica wet gel with an organic compound that is at least bifunctional and then performing drying.

7. The method of producing an aerogel blanket according to claim 5 , wherein the organic functional aerogel powder is a surface silylated aerogel powder having characteristics i) or ii) described below:
i) the surface silylated aerogel powder does not contain a Si—OR group (R is an alkyl group having 1 to 18 carbon atoms);
ii) the surface silylated aerogel powder has a degree of coverage, or a degree of cladding, of an internal surface by an organic surface group introduced through surface silylation of 90% or more, wherein the degree of coverage, or the degree of cladding, is calculated according to Equation 1:
Degree of coverage=[C]/[BET]*K; unit: [nm −2 ]  [Equation 1]

where in the above equation, K=6.022*10 23 /100*12*3*10 18 =167.28;
unit: [g- 1 ][C]: Carbon content (wt %)
[BET]: BET surface area; unit: [m 2 /gL.

8. The method of producing an aerogel blanket according to claim 1 , wherein the blanket substrate is a reinforcing structure;
wherein the reinforcing structure is a lofty fibrous batting in which fibers are oriented along all three axes;
wherein the lofty fibrous batting is in a sheet form, is compressible to at least 50% of an original thickness thereof and recoverable to at least 70% of the original thickness thereof after five seconds of compression, and has a density of 0.001 g/cm 3 to 0.26 g/cm 3 ; and
wherein a cross-sectional area of fibers identifiable from a cross-section of the aerogel blanket finally produced is less than 10% of an entire area of the cross-section of the aerogel blanket.

9. An aerogel blanket comprising an aerogel and a blanket substrate, wherein the aerogel has a carbon content retention ratio calculated according to Equation 2 and satisfies any one of 1) to 5) described below when heat-treated at a temperature equal to or greater than 400° C. and less than 500° C. for one to five hours:
Carbon content retention ratio (%)=(carbon content (wt %) in aerogel after heat treatment)/(initial carbon content in aerogel (wt %)),  [Equation 2]

1) 75% or more upon one-hour heat treatment;
2) 65% or more upon two-hour heattreatment;
3) 60% or more upon three-hour heattreatment;
4) 59% or more upon four-hour heat treatment;
5) 58% or more upon five-hour heat treatment.

10. The aerogel blanket according to claim 9 , wherein the carbon content retention ratio satisfies any one of 1) to 5) described below when heat-treated at a temperature equal to or greater than 400° C. and less than 500° C. for one to five hours:
1) 75% to 80% upon one-hour heat treatment;
2) 65% to 75% upon two-hour heattreatment;
3) 60% to 70% upon three-hour heat treatment;
4) 59% to 65% upon four-hour heat treatment;
5) 58% to 64% upon five-hour heat treatment.

11. The aerogel blanket according to claim 9 , wherein the aerogel blanket has a thermal conductivity growth rate calculated according to Equation 3 and satisfies any one of 1) to 5) described below when heat-treated at a temperature equal to or greater than 400° C. and less than 500° C. for one to five hours:
Thermal conductivity growth rate (%)=(thermal conductivity (mW/mK) of aerogel blanket at 25° C. after heat treatment)/(initial thermal conductivity (mW/mK) of aerogel blanket at 25° C.),  [Equation 3]

1) 6% or less upon one-hour heat treatment;
2) 10% or less upon two-hour heattreatment;
3) 11% or less upon three-hour heat treatment;
4) 12% or less upon four-hour heat treatment;
5) 13% or less upon five-hour heat treatment.

12. The aerogel blanket according to claim 9 , wherein the thermal conductivity growth rate satisfies any one of 1) to 5) described below when heat-treated at a temperature equal to or greater than 400° C. and less than 500° C. for one to five hours:
1) 5% to 6% upon one-hour heat treatment;
2) 7% to 10% upon two-hour heat treatment;
3) 8% to 11% upon three-hour heat treatment;
4) 9% to 12% upon four-hour heattreatment;
5) 10% to 13% upon five-hour heat treatment.

13. An aerogel blanket comprising an aerogel and a blanket substrate, wherein the aerogel has a carbon content retention ratio of 13% or more as calculated according to Equation 2 when heat-treated at a temperature of 500° C. to 600° C. for one to five hours:
Carbon content retention ratio (%)=(carbon content (wt %) in aerogel after heat treatment)/(initial carbon content in aerogel (wt %)).  [Equation 2].

14. The aerogel blanket according to claim 13 , wherein the aerogel has a carbon content retention ratio is 15% or more when heat-treated at a temperature of 500° C. to 600° C. for one to five hours.

15. The aerogel blanket according to claim 13 , wherein the carbon content retention ratio is 13% to 70% when heat-treated at a temperature of 500° C. to 600° C. for one to five hours.

16. The aerogel blanket according to claim 13 , wherein the carbon content retention ratio is 15% to 60% when heat-treated at a temperature of 500° C. to 600° C. for one to five hours.

17. The aerogel blanket according to claim 13 , wherein the carbon content retention ratio satisfies any one of 1) to 5) described below when heat-treated at a temperature of 500° C. to 600° C. for one to five hours:
1) 40% or more upon one-hour heat treatment;
2) 24% or more upon two-hour heattreatment;
3) 20% or more upon three-hour heattreatment;
4) 17% or more upon four-hour heat treatment;
5) 15% or more upon five-hour heat treatment.

18. The aerogel blanket according to claim 13 , wherein the carbon content retention ratio satisfies any one of 1) to 5) described below when heat-treated at a temperature of 500° C. to 600° C. for one to five hours:
1) 40% to 60% upon one-hour heattreatment;
2) 24% to 50% upon two-hour heattreatment;
3) 20% to 45% upon three-hour heat treatment;
4) 17% to 42% upon four-hour heat treatment;
5) 15% to 40% upon five

Assignees

• Lg Chemical Ltd

Inventors

• Kim Mi Ri
• Oh Kyoung Shil
• Lee Je Kyun
• Kim Young Hun

Classifications

• F26B21/40

  using gases other than air · CPC title

• Y10T428/30

  Self-sustaining carbon mass or layer with impregnant or other layer · CPC title

• C01B33/1585 Primary

  Dehydration into aerogels · CPC title

• D06M11/79 Primary

  with silicon dioxide, silicic acids or their salts · CPC title

• C01B33/146

  After-treatment of sols ({preparation of hydrosols or aqueous dispersions from hydroorganosols, organosols or dispersions in an organic medium C01B33/141}; preparation of hydroorganosols, organosols or dispersions in an organic medium from hydrosols {or aqueous dispersions} C01B33/145) · CPC title