Phosphor series benzoxazine and preparation method
A technology of benzocyclohexane and oxo, which is applied in the field of phosphorus-based oxonitrobenzocyclohexane and its preparation, can solve the problems of being complicated, inconvenient to operate, unsuitable for large-scale production and the like, and achieve the synthesis steps Simple, easy to process, improve the effect of poor flame resistance
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[0028] Example 1.5,5'-methylene-bis-2-hydroxybenzaldehyde synthesis
[0029] 5,5'-methylene-bis-2-hydroxybenzaldehyde is obtained by reacting 2-hydroxybenzaldehyde with trioxane, and its chemical reaction formula is:
[0030]
[0031] Its synthesis steps are as follows:
[0032] In a 0.25L three-neck reactor with a temperature indicating device, add 10g (0.111mol) of trioxane, 89.5g (0.733mol) of 2-hydroxybenzaldehyde, 100g of acetic acid and 3.09g of sulfuric acid The reaction was carried out at 85° C. for 24 hours. After the reaction, it was allowed to cool and precipitated out naturally. The precipitate was dissolved in methanol and directly poured into 1000 mL of deionized water for precipitation and washing, and filtered with a suction filter. The filter cake was dried in a vacuum oven at 110°C to obtain the product, and the yield was 40%.
[0033] The molecular formula of this product is C 15 H 12 O 4 , and its molecular weight was identified by high-resolution m...
Example Embodiment
[0034] Example 2.7,7'-Methylene-bis-[2-dihydro-3-phenyl-4-(9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) Synthesis of -4-hydroxy-1,3-oxonitrobenzocyclohexane](Bz-a)
[0035] Bz-a is obtained by the reaction of DOPO, 5,5'-methylene-bis-2-hydroxybenzaldehyde, aniline and formaldehyde. Its chemical reaction formula is:
[0036]
[0037] The synthesis steps are as follows: in a 0.25L three-neck reactor with a temperature indicating device, add 12.81g (0.05mol) of 5,5'-methylene-bis-2-hydroxybenzaldehyde, 9.3g (0.1 mol) of aniline, 100 mL of methanol and 21.6 g (0.1 mol) of DOPO were reacted at room temperature (25 °C) for 18 hours, white powder was precipitated during the reaction process, and 8.9 g (0.11 mol) was added immediately after the reaction, with a volume fraction of 37% The aqueous formaldehyde solution was first reacted at room temperature (25°C) for 4 hours, then the reaction temperature was raised to the reflux temperature, and the reaction was carried out ...
Example Embodiment
[0038] Example 3.7,7'-methylene-bis-[2-dihydro-3-n-propyl-4-(9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide )-4-hydroxy-1,3-oxoazobenzocyclohexane] (Bz-b) synthesis
[0039] Bz-b is obtained by the reaction of DOPO, 5,5'-methylene-bis-2-hydroxybenzaldehyde, propylamine and formaldehyde. Its chemical reaction formula is:
[0040]
[0041] The synthesis steps are as follows: in a 0.25L three-neck reactor with a temperature indicating device, add 12.81g (0.05mol) of 5,5'-methylene-bis-2-hydroxybenzaldehyde, 5.91g (0.1 mol) of propylamine, 100 mL of methanol and 21.6 g (0.1 mol) of DOPO were reacted at room temperature (25°C) for 18 hours, a yellow powder was precipitated during the reaction process, and 8.93 g (0.11 mol) was added immediately after the reaction. The volume fraction is 37% The aqueous formaldehyde solution was first reacted at room temperature (25°C) for 4 hours, then the reaction temperature was raised to the reflux temperature, and the reaction was carri...
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