Amino group-containing phosphate ester flame retardant and method of preparing the same
A technology of phosphoric acid esters and phosphoric acid esters, which is applied in the field of preparation of the flame retardant, and can solve the problem that it is difficult for the flame retardant to exert its flame retardant performance
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[0026] In the preparation method of the present invention, preferably, step (a) is carried out at a temperature of 0°C to 60°C for 5 to 15 hours, and step (b) is carried out at a temperature of 50°C to 100°C for 5 to 15 hours.
[0027] The alcohol used in step (a) may be selected from methanol, ethanol, propanol and butanol. However, alcohols may include (1) ethanols or (2) methanols in order to control the thermal and migration properties of the product.
[0028] The aminoalcohol used in step (b) may be selected from 2-dimethylaminoethanol, dimethylaminoethanol, 2-dimethylaminocarbinol, and 2-dimethylaminopropanol, and may preferably be 2 -Dimethylaminoethanol.
[0029] In addition, the halide amino salt used in step (b) may be selected from 2-di-chloroethylamine, 2-chloromethylethylamine, di-chloroethylamine and chloromethylethylamine, and may preferably Di-chloroethylamine.
[0030] The present invention also provides a flame retardant resin containing 5 to 50% by weight...
Embodiment 1
[0035] Embodiment 1: the preparation of three-(dimethylaminomethyl) phosphoric acid ester
[0036] At room temperature, 689.7g trichlorophosphate (POCl 3 ) was added to 1,995g of toluene, and then 640.3g of ethanol (C 2 h 5 OH), to generate 492 g of hydrogen chloride (HCl). The hydrogen chloride thus obtained was aged for 5 hours at room temperature and topped with toluene at 140°C for 5 hours, topped under reduced pressure (1 torr) at 110°C for 2 hours, and then filtered to obtain 819.3g initial reaction product triethyl phosphate (C 6 h 15 PO 4 ).
[0037] With the above-mentioned product trimethyl phosphate of 794.7g (C 3 h 9 PO 4 ) was added to 2,168 g of toluene heated up to 110° C. and 10 g of tyzor TBT. The resulting mixture was subjected to solvent reflux topping distillation while mixing dimethylaminocarbinol (C 3 h 9 NO), the dimethylaminocarbinol (C 3 h 9 NO) was added dropwise within 3 hours at 130°C to obtain 603.0g of ethanol (C 2 h 5 OH). Etha...
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