Organosilicone modified halogen-free intumescent flame retardant and preparation method thereof
An intumescent flame retardant and silicone technology, applied in the field of polymer material flame retardants, can solve problems such as limited market demand, achieve good synergistic flame retardant effect, lasting flame retardant performance, improve mechanical properties and processing. performance effect
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Embodiment 1
[0028] Add 25.2g (0.2mol) of melamine (MEL) into a four-necked flask equipped with a stirrer, a thermometer, and a condenser. The upper end of the condenser is connected to a gas absorption device, and then add 150ml of cyclohexane. 29.9 g (0.2 mol) of methyltrichlorosilane was heated, and the temperature was controlled at 45°C to stir and react for 1 hour, the temperature was raised to 60°C to continue the reaction for 1 hour, the temperature was raised to 85°C, and the reaction was refluxed for 2 hours. Stop the reaction after detecting that no hydrogen chloride gas has been released with pH test paper. Hydrogen chloride gas released during the reaction is absorbed with lye. The cyclohexane is removed by distillation under reduced pressure, and the recovered cyclohexane can be recycled. After evaporating the solvent, add 150ml of distilled water, stir and heat to 70°C for 0.5h, cool, filter, and wash with distilled water several times until there is no chloride ion in the f...
Embodiment 2
[0030]76.7g (0.3mol) melamine cyanurate (MCA) is added in the reaction system with embodiment 1, then add 200ml methylene chloride, add 29.9g (0.2mol) methyltrichlorosilane after stirring, heat , control the temperature at 45°C to reflux, and stir for 3h. The released hydrogen chloride gas is absorbed with lye. The dichloromethane (which can be recovered and reused) was removed by heating and distillation, and the temperature was raised to 90° C. to continue the reaction for 1 h, until no hydrogen chloride gas was released to stop the reaction. Slightly cold, add 150ml distilled water to continue subsequent purification measures, same as Example 1. Dry to obtain white hydrophobic powder 77.4g, yield 90.8%. The hydrophobicity of the product is the same as in Example 1. Put it in a muffle furnace and burn it at 300°C for 30 minutes without losing weight.
Embodiment 3
[0032] 67.2g (0.3mol) melamine phosphate (MP) is added in the reaction system with embodiment 1, then add 180ml acetone, add 29.9g (0.2mol) methyl trichlorosilane after stirring, heating, control temperature is Stir and react at 45°C for 1.5h, heat up to 58°C and reflux for 1.5h, and distill under reduced pressure to remove acetone. Other processing steps are the same as in Example 1. Dry to obtain product 69.7g, yield 92%, the hydrophobicity of product is the same as embodiment 1. Put it into a muffle furnace and burn at 300° C. for 30 minutes, resulting in a weight loss of 5.4%, and the weight loss of the control sample without organosilicon treatment was 4.6%.
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