A kind of ferrocene-based flame-retardant carbon-forming polymer and preparation method thereof
A ferrocene-based and polymer technology is applied in the field of ferrocene-based flame-retardant carbon-forming polymers and the preparation thereof, and can solve the problems such as the preparation method of ferrocene-based flame-retardant carbon-forming polymers that have not yet been seen, and achieve the desired result. Excellent carbon effect, excellent flame retardant, less impurity effect
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Embodiment 1
[0053] A preparation method of ferrocene-based flame-retardant carbon-forming polymer, the steps are:
[0054] Add 1 mol 1,1'-dicinnamoyl ferrocene, 1 mol p-phenylenediamine and 1 mol potassium hydroxide to the solvent toluene which is 10 times the weight of 1,1'-dicinnamoyl ferrocene under nitrogen protection, The temperature was raised to 40°C, and the reaction was carried out for 2 hours. The temperature was raised to reflux and the reaction was carried out for 12 hours. The solvent was evaporated to dryness under reduced pressure to obtain a black viscous substance, which was dispersed by adding water to obtain a light yellow substance, which was filtered and the filter cake was grinded with hydrochloric acid solution to adjust the pH to weak acidity (pH 5.0). After filtration, the filter cake was dissolved in acetone, and the dissolved solution was poured into methanol 5 times the weight of acetone to precipitate a precipitate, filtered, and dried under vacuum at 60°C to obt...
Embodiment 2
[0056] A preparation method of ferrocene-based flame-retardant carbon-forming polymer, the steps are:
[0057] Add 1 mol 1,1'-dicinnamoyl ferrocene, 1.1 mol o-phenylenediamine and 1 mol potassium hydroxide into the solvent toluene which is 12 times the weight of 1,1'-dicinnamoyl ferrocene, protected by nitrogen , The temperature is raised to 45°C, the reaction is 3h, the temperature is refluxed, and the reaction is 18h. The solvent was evaporated to dryness under reduced pressure to obtain a black viscous substance, which was dispersed by adding water to obtain a light yellow substance, which was filtered and the filter cake was grinded with hydrochloric acid solution to adjust the pH to weak acidity (pH 5.0). After filtering, the filter cake was dissolved in acetone, and the dissolved solution was poured into methanol 8 times the weight of acetone to precipitate a precipitate, filtered, and dried under vacuum at 60°C to obtain the product.
Embodiment 3
[0059] A preparation method of ferrocene-based flame-retardant carbon-forming polymer, the steps are:
[0060] Add 1mol 1,1'-dicinnamoyl ferrocene, 1.2mol m-phenylenediamine and 1mol sodium hydroxide to the solvent toluene 15 times the weight of 1,1'-dicinnamoyl ferrocene, protected by nitrogen , The temperature is increased to 50°C, the reaction is 4h, the temperature is refluxed, and the reaction is 24h. The solvent was evaporated under reduced pressure to obtain a black viscous substance, and water was added to disperse to obtain a light yellow substance, which was filtered, and the filter cake was milled and adjusted to a weakly acidic pH value with hydrochloric acid solution (pH value of 5.0). After filtering, the filter cake was dissolved with acetone, and the dissolved solution was poured into methanol 10 times the weight of acetone to precipitate a precipitate, filtered, and dried under vacuum at 60°C to obtain the product.
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Abstract
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