High temperature crosslinked flame retardant with Schiff base and phosphoryl (phosphonyl) structure, preparation method and application thereof
A technology of Schiff base and flame retardant, which is applied in the field of high-temperature cross-linking flame retardants and their preparation, can solve the problems of inability to cross-link, high molecular structure rigidity, easy aging and decomposition, etc., and achieve excellent flame retardancy and droplet resistance , reduce the concentration of free radicals, increase the effect of melt viscosity
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Embodiment 1
[0041] What this embodiment prepares is flame retardant FR1, and its reaction equation is as follows:
[0042]
[0043] Heat 30.53g of p-hydroxybenzaldehyde, 18.32g of ethanolamine, and 100mL of absolute ethanol, and reflux. As the reaction progresses, yellow precipitates gradually appear in the solution. After about 6 hours, the raw materials are basically reacted completely. Suction filtration, washing with ethanol, and drying to a shallow The yellow solid was 35.49 g, the yield was 86%, and it was recorded as monomer Ⅰ-1.
[0044] Mix 35.49g of monomer Ⅰ-1 and 63.80g of monomer Ⅱ-1, under the protection of nitrogen, stir and raise the temperature to 180°C to soften and melt the system, continue to maintain the temperature until the rod climbing phenomenon occurs, and then raise the temperature to 250°C to continue the reaction 1 h gave the product as a dark yellow solid. The hydrogen chloride gas discharged from the system is absorbed with sodium hydroxide solution. Af...
Embodiment 2
[0046] What this embodiment prepares is flame retardant FR2, and its reaction equation is as follows:
[0047]
[0048] Heat 26.04g of 3-mercaptobutyraldehyde, 15.02g of ethylenediamine and 100mL of absolute ethanol, and reflux. As the reaction progresses, a yellow precipitate gradually appears in the solution. After about 8 hours, the raw materials are basically reacted completely. Suction filtration, washing with ethanol, After drying, 29.25 g of a light yellow solid was obtained, with a yield of 80%, which was designated as monomer Ⅰ-2.
[0049] Mix 29.25g of monomer I-2, 53.99g of monomer II-1 and 2.02g of calcium chloride, under the protection of nitrogen, stir and raise the temperature to 110°C to soften and melt the system, continue to maintain the temperature until the rod climbing phenomenon occurs, and then The temperature was raised to 150° C. to continue the reaction for 5 h to obtain a dark yellow solid product. The hydrogen chloride gas discharged from the sy...
Embodiment 3
[0051] What this embodiment prepares is flame retardant FR3, and its reaction equation is as follows:
[0052]
[0053] Heat 29.04g of 2-methyl-3-methylpentanal, 22.73g of p-hydroxyaniline and 100mL of absolute ethanol, and reflux. As the reaction proceeds, a yellow precipitate gradually appears in the solution. After about 6 hours, the basic reaction of the raw materials is basically complete. Filter, wash with ethanol, and dry to obtain 37.57 g of a light yellow solid with a yield of 87%, which is designated as monomer Ⅰ-3.
[0054] Mix 37.57g of monomer I-3, 51.26g of monomer II-1 and 0.02g of aluminum chloride under the protection of nitrogen, stir and raise the temperature to 170°C to soften and melt the system, continue to maintain the temperature until the rod climbing phenomenon occurs, and then The temperature was raised to 220° C. to continue the reaction for 2 h to obtain a dark yellow solid product. The hydrogen chloride gas discharged from the system is absorb...
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