Biodegradable halogen-free flame retardant and preparation method thereof
A kind of flame retardant, biological technology, applied in the field of biodegradable halogen-free flame retardant and its preparation, to achieve the effect of environmental friendliness, wide source and excellent flame retardant performance in production and manufacturing
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Embodiment 1
[0030] (1) Preparation of phosphated chitosan: Dissolve 4g of chitosan in 60ml of methanesulfonic acid, add 20g of phosphorus pentoxide after complete dissolution, react under nitrogen protection, and continue for 3 hours in an ice-water bath at -10°C . The product after the reaction was washed with ether, acetone, and methanol respectively, and a white powder was obtained after suction filtration in a suction filtration machine. Then, put the white powder into a vacuum drying oven and dry for 24 hours to obtain the intermediate product phosphorylated chitosan.
[0031] (2) Preparation of functionalized chitosan: 4g phosphorylated chitosan is dissolved in 120ml distilled water, and after dissolving completely, a brown transparent solution is obtained, then the sodium hydroxide solution of 1.0mol / L is added dropwise in the solution, and stir until the solution is neutral. 200ml of 0.5mol / L cobalt chloride was added dropwise to the resulting neutral solution, while stirring fo...
Embodiment 2
[0035] (1) Preparation of phosphated chitosan: Dissolve 4g of chitosan in 60ml of methanesulfonic acid, add 28g of phosphorus pentoxide after complete dissolution, and react in an ice-water bath at 5° C. for 5 hours under nitrogen protection. The product after the reaction was washed with ether, acetone, and methanol respectively, and a white powder was obtained after suction filtration in a suction filtration machine. Then, put the white powder into a vacuum drying oven and dry for 24 hours to obtain the intermediate product phosphorylated chitosan.
[0036] (2) Preparation of functionalized chitosan: 4g phosphorylated chitosan is dissolved in 120ml distilled water, and after dissolving completely, a brown transparent solution is obtained, then the sodium hydroxide solution of 2.0mol / L is added dropwise in the solution, and stir until the solution is neutral. 100ml of 1mol / L cerium nitrate was added dropwise to the obtained neutral solution while stirring for 8h. After the ...
Embodiment 3
[0040] (1) Preparation of phosphated chitosan: Dissolve 4g of chitosan in 60ml of methanesulfonic acid, add 36g of phosphorus pentoxide after complete dissolution, and react in an ice-water bath at 0° C. for 8 hours under nitrogen protection. The product after the reaction was washed with ether, acetone, and methanol respectively, and a white powder was obtained after suction filtration in a suction filtration machine. Then, put the white powder into a vacuum drying oven and dry for 24 hours to obtain the intermediate product phosphorylated chitosan.
[0041] (2) Preparation of functionalized chitosan: 4g phosphorylated chitosan is dissolved in 120ml distilled water, after dissolving completely, a brown transparent solution is obtained, then the potassium hydroxide solution of 1.0mol / L is added dropwise in the solution, and stir until the solution is neutral. Add 66.67ml of 1.5mol / L ferric chloride dropwise into the resulting neutral solution while stirring for 10h. After th...
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