A kind of metal complex containing p/n/si/s/ni synergistic catalytic flame retardant and preparation method thereof
A technology of metal complexes and synergistic catalysis, applied in the field of intumescent metal flame retardants, can solve the problems of halogen-based flame retardants, such as toxic smoke, large usage, and poor flame retardant efficiency of intumescent organic flame retardants. , to achieve the effect of improving the flame retardant effect, the synthesis process conditions are mild and stable, and the reaction process is simple and easy to control.
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Embodiment 1
[0038] A preparation method of a metal complex containing P / N / Si / S / Ni synergistically catalyzed and flame-retardant is:
[0039] (1) In 30mL of dichloromethane, first add 2.3mL (10mmol) of 3-aminopropyltriethoxysilane, then slowly add 4.1mL (23mmol) of diphenylphosphorous chloride, then slowly add 3.1 mL (22 mmol) of triethylamine; after stirring overnight at room temperature, a light yellow suspension was obtained, which was filtered through a sand core to remove the triethylamine hydrochloride solid to obtain a light yellow liquid, which was rotary evaporated to remove dichloromethane to obtain Solid crude product; finally, it was washed with tetrahydrofuran, recrystallized from dichloromethane and dried in vacuo to obtain a pale white solid, namely intermediate I (yield 89%); melting point was 66-68°C.
[0040] (2) In a mixed solvent of 35mL absolute ethanol + 10mL dichloromethane, first add 1.19g (5.0mmol) of nickel dichloride hexahydrate and stir vigorously until complete...
Embodiment 2
[0045] A preparation method of a metal complex containing P / N / Si / S / Ni synergistically catalyzed and flame-retardant is:
[0046] (1) In 30mL of dichloromethane, first add 2.3mL (10mmol) of 3-aminopropyltriethoxysilane, then slowly add 4.1mL (23mmol) of diphenylphosphorous chloride, then slowly add 3.1 mL (22 mmol) of triethylamine; after stirring overnight at room temperature, a light yellow suspension was obtained, which was filtered through a sand core to remove the triethylamine hydrochloride solid to obtain a light yellow liquid, which was rotary evaporated to remove dichloromethane to obtain Solid crude product; finally, it was washed with tetrahydrofuran, recrystallized from dichloromethane and dried in vacuo to obtain a pale white solid, which is intermediate I (yield 88%).
[0047] (2) In a mixed solvent of 35mL absolute ethanol + 10mL dichloromethane, first add 1.10g (5.0mmol) of anhydrous nickel dibromide and stir vigorously until completely dissolved, then add 3.25g...
Embodiment 3
[0050] A preparation method of a metal complex containing P / N / Si / S / Ni synergistically catalyzed and flame-retardant is:
[0051] (1) In 30mL of dichloromethane, first add 2.3mL (10mmol) of 3-aminopropyltriethoxysilane, then slowly add 4.1mL (23mmol) of diphenylphosphorous chloride, then slowly add 3.1 mL (22 mmol) of triethylamine; after stirring overnight at room temperature, a light yellow suspension was obtained, which was filtered through a sand core to remove the triethylamine hydrochloride solid to obtain a light yellow liquid, which was rotary evaporated to remove dichloromethane to obtain Solid crude product; finally, it was washed with tetrahydrofuran, recrystallized from dichloromethane and dried in vacuo to obtain a pale white solid, which is intermediate I (91% yield).
[0052] (2) In a mixed solvent of 35mL anhydrous methanol + 10mL dichloromethane, first add 1.34g (5.0mmol) of anhydrous nickel diiodide and stir vigorously until completely dissolved, then add 3.25...
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