Halogen-free active fire retardant and preparation method thereof
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A flame retardant and active technology, applied in the field of halogen-free active flame retardants and their preparation, can solve problems such as environmental pollution, achieve the effects of good compatibility, high yield and easy commercial production
Active Publication Date: 2015-06-17
XIAMEN UNIV +1
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Problems solved by technology
Halogenated polyols have good flame retardant effect, but they are banned because of their environmental pollution
Method used
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Embodiment 1
[0025] Under nitrogen protection, add reactant N-hydroxyethylaniline (13.718g, 0.1mol), 4-hydroxybenzaldehyde (12.212g, 0.1mol) and 200ml of toluene, heat up to 90°C, keep the system under reflux for 2 hours, then add DOPO (21.6g, 0.1mol) and continue the reaction for 4 hours, a light blue solid precipitate can be obtained, cool down, let stand, pour off the upper solvent, and then use The solvent was washed 3 times, put into a vacuum oven at elevated temperature (60°C) and dried to obtain 42.32 g of light blue solid product DOPO-PEA, with a yield of 89.03%.
Embodiment 2
[0027] Under nitrogen protection, add reactant N-hydroxyethylaniline (7.544g, 0.055mol), 4-hydroxybenzaldehyde (6.106g, 0.05mol) and 100ml of toluene, heat up to 90°C, keep the system under reflux for 2 hours, then add DOPO (10.8g, 0.05mol) and continue the reaction for 3 hours, a light blue solid precipitate can be obtained, cool down, let stand, pour off the upper solvent, and then use The solvent was washed 3 times, put into a vacuum oven and dried at elevated temperature (50° C.) to obtain 22.02 g of light blue solid product DOPO-PEA, with a yield of 90.06%.
Embodiment 3
[0029] Under nitrogen protection, add reactant N-hydroxyethylaniline (16.462g, 0.12mol), 4-hydroxybenzaldehyde (12.212g, 0.1mol) and 200ml of toluene, heat up to 80°C, keep the system under reflux for 4 hours, then add DOPO (21.6g, 0.1mol) and continue the reaction for 4 hours, a light blue solid precipitate can be obtained, cool, let stand, pour off the upper solvent, and then use The solvent was washed 3 times, put into a vacuum oven and dried at elevated temperature (60° C.) to obtain 43.82 g of light blue solid product DOPO-PEA, with a yield of 87.17%.
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Abstract
The invention relates to fire retardants, and in particular relates to a halogen-free active fire retardant and a preparation method thereof. The method comprises the following steps: under the protection of nitrogen, sequentially adding reactants, namely N-hydroxyethylaniline, 4-hydroxybenzaldehyde and a solvent, into a container equipped with a condensate return pipe and a magnetic stirrer; after a heating reaction, adding DOPO to continue the reaction to obtain a light blue solid deposit; and cooling the deposit, keeping the deposit standing, pouring out the upper-layer solvent, washing the deposit with a solvent, and drying the deposit to obtain the halogen-free active fire retardant. Or the method comprises the following steps: under the protection of nitrogen, sequentially adding the reactants, namely N-hydroxyethylaniline, 4-hydroxybenzaldehyde and a solvent, into a container equipped with a condensate return pipe and a magnetic stirrer; after a heating reaction, adding DOPO to continue the reaction to obtain a light blue solution; and concentrating the solution, and precipitating the solution with a precipitator to obtain the halogen-free active fire retardant. The preparation method is simple, and the halogen-free active fire retardant contains a plurality of kinds of active groups, is well compatible with a matrix and has a good halogen-free flame-retardant property.
Description
technical field [0001] The invention relates to a flame retardant, in particular to a halogen-free active flame retardant and a preparation method thereof. Background technique [0002] With the development of science and technology, polymers such as polyurethane, polyester PET, PBT and epoxy resin have been widely used in transportation, electronic appliances, automobiles, engineering and other fields. In addition, the requirements for the diversification of the properties of these polymers are also increasing, and the requirements for flame retardancy are extremely important. [0003] Usually, in order to make the polymer flame retardant, flame retardants need to be added, and can be divided into additive flame retardants and active flame retardants according to the reactivity. Additive flame retardants are more commonly used, but there are disadvantages such as large amount of addition and great influence on the mechanical properties of polymers; while active flame retar...
Claims
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