A polylactic acid/starch intumescent flame-retardant composite material and its preparation method
A technology of intumescent flame retardant and composite material, which is applied in the field of polylactic acid/starch intumescent flame retardant composite material and its preparation, and can solve the problems of poor compatibility between starch and matrix plastic, poor thermal stability of starch, and inability to meet application requirements. , to achieve the effect of promoting carbon forming ability, high phosphorus content and high phosphorus content
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Embodiment 1
[0061] In a 250mL three-necked flask, 20g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 15g of maleic anhydride (MA) were dissolved in 50mL of toluene and 20mL of dioxygen Hexacyclic, heated to 40 ° C, nitrogen protection, reflux reaction for 12 hours. After the reaction, the solvent was removed by rotary evaporation, and the product 1 was obtained after vacuum drying, which was set aside.
[0062] In a 250mL three-necked flask, 20g of starch (corn starch) and 40mL of pyridine were heated to 65°C and refluxed for 2h under nitrogen protection. After the temperature dropped to 50°C, 20g of the product 1 (dissolved in DMSO) was added to the catalyst 4-dimethylaminopyridine, protected by nitrogen, and refluxed at 50°C for 12h. After the reaction is finished, it is washed, purified, and vacuum-dried to obtain bio-based phosphorus-containing starch, ie, modified starch.
Embodiment 2
[0064] In a 250mL three-necked flask, 20g DOPO and 18g maleic anhydride (MA) were respectively dissolved in 50mL xylene and 20mL THF (tetrahydrofuran), heated to 50°C, under nitrogen protection, and refluxed for 24h. After the reaction, the solvent was removed by rotary evaporation, and the product 1 was obtained after vacuum drying, which was set aside.
[0065] In a 250mL three-necked flask, 20g of starch (corn starch) and 60mL of pyridine were heated to 75°C and refluxed for 4h under nitrogen protection. After the temperature dropped to 50°C, 25g of the product 1 (dissolved in DMSO) was added to the catalyst 4-dimethylaminopyridine, protected by nitrogen, and refluxed for 24h. After the reaction is finished, it is washed, purified, and vacuum-dried to obtain bio-based phosphorus-containing starch, ie, modified starch.
Embodiment 3
[0067] In a 250mL three-necked flask, 20g DOPO and 21g maleic anhydride (MA) were dissolved in 70mL xylene, heated to 60°C, under nitrogen protection, and refluxed for 24h. After the reaction, the solvent was removed by rotary evaporation, and the product 1 was obtained after vacuum drying, which was set aside.
[0068] In a 250mL three-necked flask, 20g of starch (corn starch) and 80mL of pyridine were heated to 85°C and refluxed for 8h under nitrogen protection. After the temperature dropped to 65°C, 35g of the product 1 (dissolved in DMSO) was added to the catalyst 4-dimethylaminopyridine, protected by nitrogen, and refluxed for 24h. After the reaction is finished, it is washed, purified, and vacuum-dried to obtain bio-based phosphorus-containing starch, ie, modified starch.
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