A kind of preparation method of cage molecule modified graphene oxide flame retardant
A cage-like molecule and oxide stone technology, applied in epoxy resin coatings, coatings, fire-retardant coatings, etc., can solve the problems of toxic release, environmental pollution, secondary human injury, etc., improve the flame retardant level, and the preparation method is simple. , Easy to operate effect
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Embodiment 1
[0021] Step 1. Synthesis and purification of caged phosphate
[0022] In a 500ml three-neck flask, add 1mol pentaerythritol and 1mol phosphorus oxychloride and pour 300ml of dioxane solvent, react in a water bath at 85°C at a stirring speed of 180r / min for 3h, then raise the temperature to 93°C, and reflux for 3h , the final temperature was fixed at 95°C, and the solvent was slowly distilled off while stirring the reaction to obtain a white solid. Dissolve the above-mentioned white solid in 300ml of absolute ethanol, stir in a water bath at 80°C at a stirring speed of 120r / min until completely dissolved, filter at 25°C, cool and recrystallize, dry in vacuum at 120°C for 24 hours, and set aside.
[0023] Step 2. Acid Chloride Activation of PEPA
[0024] Take 150ml of freshly steamed dioxane in a three-necked flask, weigh 0.2mol of diacyl chloride, pour it into a flask filled with solvent, and under nitrogen protection, at a speed of 120r / min, stir electromagnetically for 8min,...
Embodiment 2
[0032] Step 1. Synthesis and purification of caged phosphate
[0033] In a 500ml three-necked flask, add 1mol of pentaerythritol and 1mol of phosphorus oxychloride and pour 350ml of dioxane solvent, react in a water bath at 85°C at a stirring speed of 180r / min for 3h, then raise the temperature to 93°C, and reflux for 3h , the final temperature was fixed at 95°C, and the solvent was slowly distilled off while stirring the reaction to obtain a white solid. Dissolve the above-mentioned white solid in 300ml of absolute ethanol, stir in a water bath at 80°C at a stirring speed of 120r / min until completely dissolved, filter at 25°C, cool and recrystallize, dry in vacuum at 120°C for 24 hours, and set aside.
[0034] Step 2. Acid Chloride Activation of PEPA
[0035] Take 150ml of freshly steamed dioxane in a three-neck flask, weigh 0.1mol of diacyl chloride, pour it into a flask filled with solvent, and under nitrogen protection, at a speed of 150r / min, stir electromagnetically for...
Embodiment 1-2
[0044] Formula and performance comparison table of embodiment 1-2 and ratio 1
[0045]
[0046] As can be seen from the performance comparison of Examples 1-2 and Comparative Example 1 in the above table, the addition of flame retardant has little effect on the surface drying time of epoxy resin; the addition of flame retardant makes the adhesion of the coating slightly weaker. decreased, but had no effect on the application of the coating; the addition of flame retardants improved the fire resistance limit time of epoxy coatings, compared with pure epoxy coatings, the fire resistance time was increased by more than 30%; the addition of flame retardants had no effect on the Oxygen coating water resistance and salt spray resistance 480h test are very small.
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