Phosphorus-containing fire retardant and preparation method thereof
A flame retardant, content technology, applied in the field of flame retardants, can solve the problems of melt dripping, flame retardant thermal stability, compatibility and low flame retardant efficiency, achieve fast reaction rate, ensure durability, good compatibility
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[0063] The preparation method of phosphorus-containing flame retardant provided by the invention, the general reaction formula is as follows:
[0064]
[0065] It includes the following steps:
[0066] (1) Add metered amounts of bisphenol A, phosphorus-containing hydroquinone derivatives, and polymerization catalyst (IPTC) into a reaction vessel containing 600 mL of aqueous sodium hydroxide solution (sodium hydroxide concentration is 0.04 g / mL) to form a uniform solution. solution;
[0067] (2) Slowly add the solution obtained in step (1) dropwise to an organic solvent containing a metered amount of triphosgene, (the content of triphosgene in the organic solvent is 0.075g / mL), and keep the solution below 15°C and dropwise add 0.5- 2 hours, after the dropwise addition is completed, keep the solution temperature at 0-30 ° C, pH value at 9-10, react for 1-3 hours, remove the aqueous phase solution, and separate the organic phase to obtain a crude phosphorus-containing flame r...
Embodiment 1
[0090] In embodiment 1, the concrete steps of preparing phosphorus-containing flame retardant are as follows:
[0091] (1) 0.068mol (15.5g) bisphenol A, 0.23mol (42.81g) dimethylphosphine-1,4-hydroquinone, 0.03mol 4-(N,N'-dimethylamino) Pyridine was added to a reaction vessel containing 600 mL of aqueous sodium hydroxide solution (sodium hydroxide concentration of 0.04 g / mL) to form a homogeneous solution;
[0092] (2) Slowly add the solution obtained in step (1) dropwise to 376 mL of an organic solvent containing 0.1 mol (28.2 g) triphosgene, (the content of triphosgene in the organic solvent is 0.075 g / mL), and keep the solution at 15 Add dropwise below ℃ for 0.5-2 hours, after the dropwise addition is completed, keep the solution temperature at 10-30 °C, pH value at 9-10, react for 1-3 hours, remove the aqueous phase solution, and separate the organic phase to obtain crude Phosphorus flame retardant;
[0093] (3) The crude product obtained in step (2) was washed with distil...
Embodiment 2
[0103] In Example 2, the phosphoryl hydroquinone carbonate copolymer was prepared according to the above method, and the consumption of the raw materials was determined according to the molar ratio shown in Table 1,
[0104] The molar ratio of bisphenol A to DMPP was 45:55; the molar ratio of the sum of bisphenol A and DMPP to triphosgene was 100:33; and the molar ratio of polymerization catalyst to triphosgene was 15:33.
[0105] Similarly, in theory, in the phosphoryl hydroquinone carbonate copolymer prepared in Example 2, (m+p):o=1:1; p:m=0.8:1; the moles of polymerization catalyst and triphosgene The ratio is 0.45:1.
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Abstract
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