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US4873218A Expired / Lapsed US ⏱️ 0.0 years remaining

Low density, resorcinol-formaldehyde aerogels

Assignee: Lawrence Livermore National Security LLC
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Filing: 1988-05-26
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Granted: 1989-10-10
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Expires: 2008-05-26
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Abstract

Abstract The polycondensation of resorcinol with formaldehyde under alkaline conditions results in the formation of surface functionalized polymer "clusters". The covalent crosslinking of these "clusters" produces gels which when processed under supercritical conditions, produce low density, organic aerogels (density ≦100 mg/cc; cell size ≦0.1 microns). The aerogels are transparent, dark red in color and consist of interconnected colloidal-like particles with diameters of about 100 Å. These aerogels may be further carbonized to form low density carbon foams with cell size of about 0.1 micron.

Inventors

  • 👤 Richard W. Pekala

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 20:33
CPC Classifications
C; C08; C08G; C08G8/00; C08G8/04; C08G8/08; C08G8/20; B; B01; B01J; B01J20/00; B01J20/02; B01J20/20

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 83 words
A process for the synthesis of a low density, organic aerogel of ultra-fine pore size, said process comprising the steps of: mixing in a predetermined ratio a polyhydroxy benzene and formaldehyde in the presence of a base catalyst; heating the mixture to a predetermined temperature for a sufficiently long period of time to form a stable gel; washing the gel in a suitable organic solvent to exchange the aqueous solvent for the organic solvent; critical point drying the gel; and characterizing the gel.
Claim 2
Dependent Claim 83 words
A process for the synthesis of a low density, organic aerogel of ultra-fine pore size, said process comprising the steps of: mixing in a predetermined ratio a polyhydroxy benzene and formaldehyde in the presence of a base catalyst; heating the mixture to a predetermined temperature for a sufficiently long period of time to form a stable gel; washing the gel in a suitable organic solvent to exchange the aqueous solvent for the organic solvent; critical point drying the gel; and characterizing the gel.
Claim 3
Dependent Claim 21 words
The process of claim 1, wherein the pH of said mixture is in the range of about 6.5 to about 7.4.
Claim 4
Dependent Claim 13 words
The process of claim 2, wherein the polyhydroxy benzene is a dihydroxy benzene.
Claim 5
Dependent Claim 25 words
The process of claim 3, wherein said dihydroxy benzene is selected from the group consisting of resorcinol, catechol, substituted resorcinol, substituted catechol and mixtures thereof.
Claim 6
Dependent Claim 11 words
The process of claim 4, wherein said dihydroxy benzene is resorcinol.
Claim 7
Dependent Claim 21 words
The process of claim 5, wherein said solvent is selected from the group consisting of methanol, acetone, isopropanol and amyl acetate.
Claim 8
Dependent Claim 10 words
The process of claim 6, wherein said solvent is acetone.
Claim 9
Dependent Claim 17 words
The process of claim 7, wherein the ratio of said resorcinol to said formaldehyde is about 1:2.
Claim 10
Dependent Claim 12 words
The process of claim 8, wherein said base catalyst is sodium carbonate.
Claim 11
Dependent Claim 41 words
The process of claim 9, further comprising the step of heating said aerogel in a nitrogen atmosphere, to a temperature in the range of about 600° to about 1200° C. to carbonize said aerogel and form a low density, carbon foam.
Claim 12
Dependent Claim 16 words
The process of claim 4, wherein said dihydroxy benzene is a mixture of resorcinol and catechol.
Claim 13
Dependent Claim 16 words
The process of claim 4, wherein said dihydroxy benzene is a mixture of resorcinol and hydroquinone.
Claim 14
Dependent Claim 16 words
The process of claim 4, wherein said dihydroxy benzene is a mixture of resorcinol and phloroglucinol.
Claim 15
Dependent Claim 173 words
A process for the synthesis of a low density, microcellular resorcinol-formaldehyde aerogel, said process comprising the steps of: (a) mixing resorcinol and formaldehyde in a molar ratio of about 1:2, in the presence of catalytic amounts of sodium carbonate; (b) adjusting the pH of the mixture to a value in the range of about 6.5 to about 7.4; (c) decanting the mixture into a glass ampoule; (d) sealing the glass ampoule; (e) heating the mixture to about 85° C. in an oven for about seven days to facilitate formation of a gel; (f) removing the ampoule from the oven and cooling it to room temperature; (g) breaking the ampoule and removing the gel from the ampoule; (h) washing the gel in an agitated bath of trifluoracetic acid at 45° C. for three days; (i) transferring the gel from the acid bath to an agitated acetone bath maintained at about 45° C., to remove water; (j) removing the gel from the acetone bath and critical point drying the gel; and (k) characterizing the gel.
Claim 16
Dependent Claim 173 words
A process for the synthesis of a low density, microcellular resorcinol-formaldehyde aerogel, said process comprising the steps of: (a) mixing resorcinol and formaldehyde in a molar ratio of about 1:2, in the presence of catalytic amounts of sodium carbonate; (b) adjusting the pH of the mixture to a value in the range of about 6.5 to about 7.4; (c) decanting the mixture into a glass ampoule; (d) sealing the glass ampoule; (e) heating the mixture to about 85° C. in an oven for about seven days to facilitate formation of a gel; (f) removing the ampoule from the oven and cooling it to room temperature; (g) breaking the ampoule and removing the gel from the ampoule; (h) washing the gel in an agitated bath of trifluoracetic acid at 45° C. for three days; (i) transferring the gel from the acid bath to an agitated acetone bath maintained at about 45° C., to remove water; (j) removing the gel from the acetone bath and critical point drying the gel; and (k) characterizing the gel.
Claim 17
Dependent Claim 41 words
The process of claim 14, further comprising the step of heating said aerogel in a nitrogen atmosphere to a temperature in the range of about 600° to about 1200° C. to carbonize said aerogel and form a low density, carbon foam.

References Cited (Backward Citations)

US4221873A Cited
US4409361A Cited
US4336170A Cited
US4309527A Cited

USPTO Annuity & Maintenance Windows

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