Preparation method of composite flame retardant pretreatment liquid
A pretreatment liquid and composite flame retardant technology, which is applied in the field of foam plastic modification, can solve the problems of large amount of flame retardant added, environmental and human hazards, and inability to effectively exert the flame retardant effect, so as to improve the flame retardant performance Effect
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Embodiment 1
[0030] A preparation method of a composite flame-retardant pretreatment liquid, the preparation method comprising the following preparation steps:
[0031] a) Add methyl p-toluenesulfonate and 2-ethyl-4,5-dihydrooxazoline to anhydrous acetonitrile to prepare a mixed solution, the concentration of methyl p-toluenesulfonate in the mixed solution is 0.2mmol / L , the concentration of 2--ethyl-4,5-dihydrooxazoline is 1.05mmol / L, the mixture is ultrasonically oscillated for 20min, then heated at 80°C for 48h, and the solvent is evaporated to dryness to obtain a powder ;
[0032]b) Add the powder obtained in step a) into 18wt% hydrogen chloride solution, the mass ratio of the used powder to the hydrogen chloride solution is 15:18, stir for 15 minutes, then place it at 100°C for 24 hours, and rotate to evaporate Slowly add saturated sodium hydroxide solution dropwise to the remaining dry liquid, control its pH value to 9, wait for 5 minutes after the white precipitate is formed, filte...
Embodiment 2
[0037] A preparation method of a composite flame-retardant pretreatment liquid, the preparation method comprising the following preparation steps:
[0038] a) Add methyl p-toluenesulfonate and 2-ethyl-4,5-dihydrooxazoline to anhydrous acetonitrile to prepare a mixed solution, the concentration of methyl p-toluenesulfonate in the mixed solution is 0.3mmol / L , the concentration of 2--ethyl-4,5-dihydrooxazoline is 1.35mmol / L, the mixture is ultrasonically oscillated for 25min, then heated at 85°C for 50h, and the solvent is evaporated to dryness to obtain a powder ;
[0039] b) Add the powder obtained in step a) into 19wt% hydrogen chloride solution, the mass ratio of the used powder to the hydrogen chloride solution is 15:22, stir for 20 minutes, place it at 115°C for 26 hours, and rotate to evaporate Slowly add saturated sodium hydroxide solution dropwise to the remaining dry liquid, control its pH value to 10, wait for 10 minutes after the white precipitate is formed, filter ...
Embodiment 3
[0044] A preparation method of a composite flame-retardant pretreatment liquid, the preparation method comprising the following preparation steps:
[0045] a) Add methyl p-toluenesulfonate and 2-ethyl-4,5-dihydrooxazoline to anhydrous acetonitrile to prepare a mixed solution, the concentration of methyl p-toluenesulfonate in the mixed solution is 0.3mmol / L , the concentration of 2--ethyl-4,5-dihydrooxazoline is 1.05mmol / L, the mixture is ultrasonically oscillated for 25min, then heated at 80°C for 48h, and the solvent is evaporated to dryness to obtain a powder ;
[0046] b) Add the powder obtained in step a) into 18t% hydrogen chloride solution, the mass ratio of the powder used to the hydrogen chloride solution is 15:20, stir for 20 minutes, place it at 110°C for 24 hours, and rotate to evaporate Slowly add saturated sodium hydroxide solution dropwise to the remaining dry liquid, control its pH value to 9, wait for 5 minutes after the white precipitate is formed, filter to ...
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