Benzoxazine based copolymer aerogels
A benzoxazine and copolymer technology, applied in the field of benzoxazine-based copolymer aerogels, can solve the problems of collapse, low thermal conductivity, brittleness and the like
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Embodiment 1
[0187] Benzoxazine-anhydride airgel; with or without catalyst
[0188] Using 6,6'-(2,2-propanediyl)bis(3-phenyl-3,4-dihydro-2H-1,3-benzoxazine) (Ba-Bz) from Huntsman and from Sigma Aldrich's benzophenone tetracarboxylic dianhydride (4,4-BTDA) for the preparation of polybenzoxazine-anhydride airgel.
[0189] Solutions with a total solids content of about 10% by weight were prepared from the two solutions. For the first solution, Ba-Bz (1.10 g, 2.4 mmol) and 4,4-BTDA (0.12 g, 0.38 mmol) were dissolved in 5 mL of dimethylsulfoxide (DMSO). The mixture had a benzoxazine / anhydride weight ratio of 9:1 (90:10% by weight). A second solution was prepared by dissolving iron(III) acetylacetonate (0.084 g, 0.24 mmol) in 5 mL DMSO. The two solutions were mixed, transferred to sealed molds and heated at 130°C (62 hours). The gel was washed stepwise with DMSO (2x), DMSO:acetone (1:1, 2x), and acetone (6x), each step was 12 hours, and an amount three times the volume of the gel was used. ...
Embodiment 2
[0196] Except 3,3',4,4'-biphenyltetracarboxylic dianhydride (S-BDPA) is used as the dianhydride of Sigma Aldrich and 4,4'-bis(3,4-dihydro-2H-1, 3-Benzoxazin-3-yl)phenylmethane (PdBz) was used as Henkel's bisbenzoxazine, and aerogels were prepared using the method described above without the addition of catalysts.
[0197]
Embodiment 3
[0199] Polybenzoxazine-epoxy airgel. Dibenzoxazine
[0200] Using 6,6'-(2,2-propanediyl)bis(3-phenyl-3,4-dihydro-2H-1,3-benzoxazine) (Ba-Bz) from Huntsman and 1 , 1,2,2-tetra(hydroxyphenyl)ethane tetraglycidyl ether (XB-4399-3) prepared polybenzoxazine-epoxy airgel.
[0201] Solutions with a total solids content of about 10% by weight were prepared from the two solutions. For the first solution, Ba-Bz (1.10 g, 2.4 mmol) and XB-4399-3 (0.12 g, 0.20 mmol) were dissolved in 5 mL of dimethylsulfoxide (DMSO). The mixture had a benzoxazine / epoxy weight ratio of 9:1 (90:10% by weight). A second solution was prepared by dissolving 4,4'-thiobisphenol (0.12 g, 0.56 mmol) in 5 mL DMSO. The two solutions were mixed, transferred into sealed molds and heated at 130°C (100 hours) and 150°C (5 hours). The gel was washed stepwise with DMSO (2x), DMSO:acetone (1:1, 2x), and acetone (6x), each step was 12 hours, and an amount three times the volume of the gel was used. Finally, the we...
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