Benzoxazines and compositions containing benzoxazines
A technology of benzoxazine and composition, which is applied in the field of benzoxazine and benzoxazine-containing composition, and can solve problems such as difficult processing
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example 1
[0071] Liquid monofunctional benzoxazines were prepared by:
[0072] 1. Weigh 18.68 grams of phenol, 20.94 grams of amine, and 20.76 grams of paraformaldehyde, then mix in a glass bottle at room temperature (about 20.0° C.) for 20 minutes.
[0073] 2. Stir the blended materials while placing the glass jar in an oil bath heated to 115°C for 40 minutes.
[0074] 3. The temperature of the oil bath was raised to 120°C and stirring was continued for another 20 minutes.
[0075] 4. Remove the glass bottle from the oil bath and allow to cool for about 5 minutes. The blended materials were then slowly added to 10 mL of ether with stirring. The mixture was then stirred at room temperature (approximately 20.0° C.) for an additional 20 minutes.
[0076] 5. After stirring, the benzoxazine-ether mixture was washed three times with 2.0M NaOH aqueous solution in a separatory funnel, 100 ml each.
[0077] 6. After adding NaOH, wash with water to neutralize the pH (pH7).
[0078] 7. The m...
example 2
[0095] Compare
[0096] For comparison, an alkylated liquid benzoxazine without electron-withdrawing groups was formed from m-cresol, m-toluidine, and paraformaldehyde using the method described in Example 1. The alkylated liquid benzoxazine has the following structure:
[0097]
[0098] Figure 4 The resulting DSC activation energy curve and reactivity table for this alkylated liquid benzoxazine are shown. From Figure 4 ,and Figure 3A-3B Compared to the data shown for halogenated liquid benzoxazines, higher activation energies and lower conversions can be seen.
[0099] Alkylated liquid benzoxazine and bisphenol-A benzoxazine blends are based on 95:5, 90:10, 80:20 and 50:50 bisphenol-A benzoxazine:alkyl The weight ratio of liquid benzoxazine is formed. The blend was then cured according to the cure cycle described in Example 1. Figure 5 The cured blend is shown. Figure 5 It was shown that, when cured with bisphenol-A benzoxazines, the stability level of alkylat...
example 3
[0109] sticky test
[0110] Preparation of bisphenol-A benzoxazine / epoxy resin blend, bisphenol-A benzoxazine / fluorinated liquid benzoxazine blend, bisphenol-A benzoxazine / chlorinated liquid Benzoxazine blend-based samples were degassed in a vacuum oven at 110°C. After removal, it was allowed to cool to 80°C and the thumbtack test (thumb placed on the sample) was performed when the material had cooled to 25°C. As a control, pure bisphenol-A benzoxazine was also subjected to the same degassing conditions and thumb stick test. Table 3 shows the data collected on the test samples.
[0111] table 3
[0112]
[0113] As can be seen from Table 3, the uncured T of the halogenated benzoxazine system g Lower than pure BPA benzoxazine and BPA benzoxazine / epoxy blends. This uncured T g The decrease in is related to the ductility of the uncured sample. In order to make the benzoxazine-based uncured material have good ductility, the uncured T g Should be at or below room tempera...
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