Phosphorus-containing flame retardant and preparation method thereof
A technology of flame retardant and catalyst, which is applied in the field of flame retardant and its preparation, can solve problems such as unsuitable for use, unsuitable for high-frequency circuit substrates, poor reactivity of functional groups, etc., to achieve environmental protection, excellent durability, Apply a wide range of effects
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[0020] The present invention also provides a preparation method of the above-mentioned phosphorus-containing flame retardant, which includes the following steps: Step 1, reacting DOPO and quinone at 80-120°C to generate DOPO-HQ or DOPO-NQ, the molar ratio of DOPO and quinone The ratio is 1:0.6~4, and the reaction time is 1~8 hours; step 2, dissolve DOPO-HQ or DOPO-NQ in the alkali solution, stir and react, so that the -OH in DOPO-HQ or DOPO-NQ React with a base to form a salt, the molar ratio of DOPO-HQ or DOPO-NQ to the base is 1:2 to 8; step 3, add a reactive monomer with an allyl group or a reactive monomer with a vinyl group, in the presence of the catalyst Under the action, react at 60-110°C to generate the phosphorus-containing flame retardant represented by the structural formula (I), DOPO-HQ or DOPO-NQ and reactive monomers with allyl groups or reactive monomers with vinyl groups The volume molar ratio is 1:0.6-5, the molar ratio of DOPO-HQ or DOPO-NQ to the catalyst i...
Embodiment 1
[0029] (1) Synthesis of DOPO-HQ
[0030] Add 1mol (216g) DOPO and 500mL toluene to a 1000mL four-neck flask under nitrogen protection, heat and stir to 70°C, after DOPO is completely dissolved in toluene, add 0.9mol (97g) p-benzoquinone within 1.5 hours, and then The reaction was stirred at °C for 2 hours. Cool the obtained precipitate to room temperature, filter, wash with toluene several times, and dry for about 10 hours to obtain a white powder, then reconstitute the product with ethanol, and obtain white DOPO-HQ after drying, with a yield of more than 85%.
[0031] (2) Synthesis of Flame Retardant (II)
[0032]Add 324g (1mol) DOPO-HQ and 160g aqueous sodium hydroxide solution (50% concentration) in a 1 liter three-necked flask equipped with temperature controller, stirring device, cooling device and dropping funnel and stir the mixture until completely dissolved and Heat to 75°C. 137.3 g (0.9 mol) of chloromethylstyrene, 0.818 g of tetrabutylammonium bromide, and 400 g ...
Embodiment 2
[0034] (1) Synthesis of DOPO-NQ
[0035] 1 mol of DOPO and 0.9 mol of 1,4-naphthoquinone were obtained according to the synthesis method in Example 1 (1).
[0036] (2) Synthesis of Flame Retardant (III)
[0037] Add 374g (1mol) DOPO-NQ and 160g aqueous sodium hydroxide solution (50% concentration) in a 1 liter three-necked flask equipped with temperature controller, stirring device, cooling device and dropping funnel and stir the mixture until completely dissolving and Heat to 75°C. 137.3 g (0.9 mol) of chloromethylstyrene, 0.907 g of tetrabutylammonium bromide, and 400 g of toluene were mixed. The mixture solution was added dropwise over a period of 20 minutes and stirred at 75°C for a further 4 hours. Then, the solution in the flask was neutralized with 10% hydrochloric acid aqueous solution, a large amount of methanol was added to wash and precipitate the product, and the product was collected by filtration. The resultant was washed three times with a solution of methan...
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