A kind of polysilicon aluminum carbon nitrogen ceramic microsphere and its preparation method and application
A technology of polysilicon aluminum carbon nitride ceramics and polysilicon aluminazane, which is applied in coatings, anti-corrosion coatings, fire-retardant coatings, etc. Effect
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Embodiment 1
[0046] Example 1: Preparation of a novel polysilicon-aluminum-carbon-nitride ceramic microsphere
[0047](1) Preparation of liquid polysilazane: Repeatedly evacuate the Schlenk reaction bottle and fill it with argon for more than three times to ensure that the air and moisture in the bottle are removed. Anhydrous toluene 200mL, purified methylvinyldichlorosilane 20mL (21.6g) and methyldichlorosilane 16mL (17.6g), high-purity ammonia gas (99.9999%) was introduced at 0°C at 120mL / min After decomposing for 2 hours, react for 2 hours under the protection of argon flow atmosphere, and then filter in a vacuum glove box with argon atmosphere to remove the filter cake to obtain a somewhat viscous pale white liquid. The solvent is distilled off under reduced pressure at 75°C to obtain a viscous liquid Polysilazane; the above reactions are carried out under the protection of inert gases such as argon or nitrogen.
[0048] (2) Preparation of polysilazane: under argon protection at 0°C, ...
Embodiment 2
[0052] Example 2: Preparation of a novel silicon aluminum carbon nitrogen ceramic microsphere
[0053] (1) Preparation of liquid polysilazane: Repeatedly evacuate the Schlenk reaction bottle and fill it with argon for more than three times to ensure that the air and moisture in the bottle are removed. After 10 minutes of argon flow, add 200 mL of anhydrous toluene sequentially with a syringe, and then Add 20mL of purified methylvinyldichlorosilane, 8mL (8.8g) of methylvinyldichlorosilane, pass high-purity ammonia (99.9999%) at 120mL / min at 0°C for 2 hours, and then React under protection for 1 h; then filter in a vacuum glove box in an argon atmosphere to remove the filter cake to obtain a viscous pale white liquid, distill off the solvent under reduced pressure at 60-90°C to obtain viscous liquid polysilazane; Under the protection of inert gas such as argon or nitrogen;
[0054] (2) Preparation of polysilaluminazane: react under the protection of argon, slowly add 12.5 mL of...
Embodiment 3
[0058] Example 3: Preparation of a novel silicon-aluminum-carbon-nitrogen ceramic microsphere
[0059] (1) Preparation of polysilazane: consistent with step (1) and step (2) in Example 1;
[0060] (2) Preparation of polysilicon aluminum carbon nitrogen microspheres: Dissolve 0.23 g of OP-10 in 20 g of acetonitrile, and gradually add 2 g of the prepared polysilazane to the above solution dropwise under air atmosphere, and cover Cover, place on a magnetic stirrer and stir at 300rpm for 30min, then ultrasonically disperse at 30kHz for 60min to obtain a uniform emulsion. The obtained homogeneous emulsion was poured into a polytetrafluoroethylene-lined autoclave, and cured in a constant temperature oven at 180° C. for 6 hours. After the reaction, the product was equally divided into 10mL centrifuge tubes, separated by an electric centrifuge, and washed 3 times with anhydrous toluene. The sample after centrifugation was freeze-dried to obtain a yellow dry powder, namely polysilico...
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