Silicon-phosphorus synergistic coal flame-retardant dust suppressant and preparation method thereof
A technology of phosphorus-based flame retardants and silicon-based flame retardants, which is applied in the field of silicon-phosphorus synergistic coal flame retardant and dust suppressants and its preparation, can solve problems such as poor compression resistance, high cost, and fragility, and achieve resource Abundant, inexpensive, and biocompatible results
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Embodiment 1
[0069] A preparation method of silicon-phosphorus synergistic coal flame retardant and dust suppressant, comprising the following steps:
[0070] (1) Add 0.20g DOPO, 0.25g KH570 and 30.0g absolute ethanol to a three-necked flask filled with inert gas to obtain solution A;
[0071] Dissolve 0.014g of azobisisobutyronitrile in 10.0g of absolute ethanol to obtain solution B;
[0072] Add solution B to solution A dropwise for 30 minutes, then react in an oil bath at 75°C for 12 hours to obtain a crude product, remove the solvent by rotary evaporation, and then dry it for 24 hours to obtain a flame retardant intermediate.
[0073] The reaction scheme is as follows figure 1 As shown, the active hydrogen on DOPO can undergo free radical addition reaction with the double bond on KH570, and the catalyst azobisisobutyronitrile is added to accelerate the reaction, and the flame retardant intermediate is obtained from the reaction. The catalyst cannot be added too fast, otherwise it is ...
Embodiment 2
[0084] A preparation method of silicon-phosphorus synergistic coal flame retardant and dust suppressant, comprising the following steps:
[0085] (1) Add 0.20g DOPO, 0.30g KH570 and 50.0g toluene into a three-necked flask filled with inert gas to obtain solution A;
[0086] Dissolve 0.015g of azobisisobutyronitrile in 10.0g of toluene to obtain solution B;
[0087] Add solution B dropwise to solution A for 40 minutes, then react in an oil bath at 120°C for 12 hours to obtain a crude product, remove the solvent by rotary evaporation, and then dry it for 24 hours to obtain a flame retardant intermediate;
[0088] (2) Add a flame retardant intermediate to a beaker, add 57.0 g of ethanol and 3.0 g of deionized water to the flame retardant intermediate, add 0.12 g of acetic acid to adjust the pH to 4.0, and ultrasonically hydrolyze for 2 hours to obtain solution C;
[0089] Then transfer to a three-necked flask with an inert gas, add 50.0g parts of absolute ethanol, 0.20g nanomete...
Embodiment 3
[0096] A preparation method of silicon-phosphorus synergistic coal flame retardant and dust suppressant, comprising the following steps:
[0097] (1) Add 0.15g DOPO, 0.20g KH570, and 50.0g toluene into a three-necked flask filled with inert gas to obtain solution A;
[0098] Dissolve 0.011g of azobisisobutyronitrile in 10.0g of toluene to obtain solution B;
[0099] Add solution B dropwise to solution A for 40 minutes, then react in an oil bath at 120°C for 12 hours to obtain a crude product, remove the solvent by rotary evaporation, and then dry it for 24 hours to obtain a flame retardant intermediate;
[0100] (2) Add a flame retardant intermediate to a beaker, add 57.0 g of ethanol and 3.0 g of deionized water to the flame retardant intermediate, add 0.12 g of acetic acid to adjust the pH to 4.0, and ultrasonically hydrolyze for 2 hours to obtain solution C;
[0101] Then transfer to a three-necked flask with an inert gas, add 50.0g of absolute ethanol and 0.20g of kaolin,...
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