A kind of high heat-resistant organic montmorillonite flame retardant and preparation method thereof
A technology of organic montmorillonite and inorganic montmorillonite, applied in the field of flame retardant materials, can solve the problem that the heat resistance effect is not very ideal, and achieve the effect of easy to achieve large-scale, high heat resistance and high flame retardant performance
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Embodiment 1
[0039] Embodiment 1: Preparation of liquid crystal cationic quaternary ammonium salt: N,N,N-tris(2-hydroxyethyl)-N-dodecyl ammonium bromide (abbreviated as THDAB)
[0040] Add 200mL of absolute ethanol, 100mL (0.417mol) of bromododecane, and 160mL (1.669mol) of diethanolamine into a 500mL three-necked flask with a reflux condenser, react at 60°C for 48h; cool to room temperature, and pour into the reaction flask Add 20 g (0.5 mol) of sodium hydroxide to the mixture, then continue to stir the reaction at room temperature for 1 h; end the reaction, remove ethanol by rotary evaporation, add 150 mL of water to the residue, stir, then extract 3 times with 100 mL of ether, and combine the ether extracts , washed with water twice, then dried with anhydrous magnesium sulfate, filtered, and the filtrate was distilled off under reduced pressure to remove ether to obtain a colorless viscous liquid dodecyldiethanolamine;
[0041] Add dodecyldiethanolamine and 20mL (0.282mol) of 2-bromoeth...
Embodiment 2
[0042] Embodiment 2: Preparation of high heat-resistant organic montmorillonite flame retardant of the present invention
[0043] 1) Take 30g of inorganic montmorillonite and add it into deionized water to prepare a suspension with a mass fraction of 5%;
[0044] 2) Place the obtained suspension in a constant temperature water bath, take 6g of liquid crystal cationic quaternary ammonium salt: THDAB and add it to the suspension, after the addition is completed, carry out a stirring reaction at 60°C for 8 hours; finish the reaction, filter, and use deionized water Wash the filter cake until no bromide ions exist; dry the filter cake at 80°C to obtain organic montmorillonite modified by THDAB intercalation;
[0045]3) Take 30 g of organic montmorillonite modified by THDAB intercalation and place it in a three-necked flask, add 200 mL of potassium hydroxide aqueous solution with a mass fraction of 60%, stir vigorously at room temperature for 1 hour, and prepare a suspension;
[0...
Embodiment 3
[0052] Embodiment 3: Preparation of high heat-resistant organic montmorillonite flame retardant of the present invention
[0053] 1) Take 30g of inorganic montmorillonite and add it into deionized water to prepare a suspension with a mass fraction of 5%;
[0054] 2) Place the obtained suspension in a constant temperature water bath, take 8g of liquid crystal cationic quaternary ammonium salt: THDAB and add it into the suspension, after the addition is completed, carry out a stirring reaction at 65°C for 7 hours; finish the reaction, filter, and use deionized water Wash the filter cake until no bromide ions exist; dry the filter cake at 80°C to obtain organic montmorillonite modified by THDAB intercalation;
[0055] 3) Take 30 g of organic montmorillonite modified by THDAB intercalation and place it in a three-necked flask, add 200 mL of potassium hydroxide aqueous solution with a mass fraction of 60%, stir vigorously at room temperature for 1 hour, and prepare a suspension;
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