Phosphorus-containing fire retardant and preparation method thereof

[0061] The preparation method of phosphorus-containing flame retardant provided by the invention, general reaction formula is as follows:

[0062]

[0063] Including the following steps:

[0064] (1) Add measured bisphenol A, phosphorus-containing hydroquinone derivatives, and a polymerization catalyst (IPTC) into a reaction vessel containing 600 mL of sodium hydroxide aqueous solution (sodium hydroxide concentration is 0.04 g / mL) to form a uniform solution;

[0065] (2) Slowly add the solution obtained in step (1) dropwise into an organic solvent containing metered triphosgene (the content of triphosgene in the organic solvent is 0.075g / mL), keep the solution below 15°C and drop 0.5- After 2 hours, after the dropwise addition, keep the solution temperature at 0-30°C, pH value at 9-10, react for 1-3 hours, remove the aqueous phase solution, separate the organic phase, and obtain a crude phosphorus-containing flame retardant;

[0066] (3) The crude product obtained in ste

[0087]In Example 1, the specific steps for preparing a phosphorus-containing flame retardant are as follows:

[0088] (1) 0.068mol (15.5 grams) of bisphenol A, 0.23mol (42.81 grams) of dimethylphosphine-1,4-hydroquinone, 0.03mol of 4-(N,N'-dimethylamino) Pyridine was added into a reaction vessel containing 600mL aqueous sodium hydroxide solution (sodium hydroxide concentration was 0.04g / mL) to form a homogeneous solution;

[0089] (2) The solution obtained in step (1) is slowly added dropwise to 376mL of organic solvent containing 0.1mol (28.2 grams) of triphosgene, (the content of triphosgene in the organic solvent is 0.075g / mL), keep the solution at 15 Add dropwise for 0.5-2 hours below ℃, after the dropwise addition, keep the solution temperature at 10-30°C, pH value at 9-10, react for 1-3 hours, remove the aqueous phase solution, separate the organic phase, and obtain the crude product containing Phosphorus flame retardant;

[0090] (3) The crude product obtained in ste

[0100] In embodiment 2, prepare phosphoryl hydroquinone carbonate copolymer according to the above-mentioned method, determine the consumption of raw material according to the molar proportion shown in table 1,

[0101] The molar ratio of bisphenol A to DMPP is 45:55; the molar ratio of the sum of bisphenol A and DMPP to triphosgene is 100:33; the molar ratio of polymerization catalyst to triphosgene is 15:33.

[0102] In the same way, in theory, in the phosphoryl hydroquinone carbonate copolymer prepared in Example 2, (m+p): o=1: 1; p: m=0.8: 1; the mole of polymerization catalyst and triphosgene The ratio is 0.45:1.