Intumescent flame retardant and preparation method thereof
A technology of intumescent flame retardant and ammonium poly(methylidene phosphonate), which is applied in the field of flame retardants, can solve the problems of APP flame retardants such as easy moisture return, uneven dispersion, precipitation, etc., and achieves good hydrolysis stability and thermal stability. Good, simple craftsmanship
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Embodiment 1
[0027] The preparation of embodiment 1 aminotrimethylene ammonium phosphonate
[0028] It is prepared from 50% aminotrimethylene phosphonic acid and 25% industrial ammonia as raw materials. According to phosphonate PO 3 h 2 with amino NH 2 The molar ratio is 1:2.5 (aminotrimethylene phosphonic acid: ammonia=1:7.5), prepare aminotrimethylene phosphonic acid and strong ammonia water, first dilute 25% strong ammonia water to 10% (add 2 / 3 times quality of water), and then added dropwise to aminotrimethylene phosphonic acid under stirring, controlling the reaction temperature at 20-30°C, continuing to stir and react for 0.5h after the dropwise addition, heating and evaporating most of the water in the reaction mixture, and cooling to crystallize , filtered, washed, and the filtrate recovery sleeve is used to dilute concentrated ammonia water, and the filter cake is dried and crushed to obtain the ammonium trimethylene phosphonate product.
Embodiment 2
[0029] The preparation of embodiment 2 ethylenediamine tetramethylene ammonium phosphonate
[0030] It is prepared from 28% ethylenediamine tetramethylene phosphonic acid and solid ammonium bicarbonate. According to phosphonate PO 3 h 2 with amino NH 2 The molar ratio is 1:2.1 (ethylenediaminetetramethylenephosphonic acid: ammonium bicarbonate = 1:8.4), to prepare ethylenediaminetetramethylenephosphonic acid and ammonium bicarbonate, first dissolve ammonium bicarbonate in water to prepare 20% solution (add 4 times the mass of water), then add dropwise to ethylenediaminetetramethylenephosphonic acid under stirring, control the reaction temperature at 60-70°C, raise the temperature to 80-90°C after the addition and continue stirring React for 1 hour, heat to evaporate most of the water in the reaction mixture, cool to crystallize, filter, wash, and the filtrate recovery sleeve is used to prepare ammonium bicarbonate solution, the filter cake is dried and pulverized to obtain ...
Embodiment 3 2
[0031] The preparation of embodiment 3 diethylene triamine ammonium pentamethylene phosphonate
[0032] It is prepared from diethylenetriaminepentamethylenephosphonic acid with a content of 50% and solid ammonium carbonate as raw materials. According to phosphonate PO 3 h 2 with amino NH 2 The molar ratio is 1:2.2 (diethylenetriaminepentamethylenephosphonic acid: ammonium carbonate=1:5.5), prepare diethylenetriaminepentamethylenephosphonic acid and ammonium carbonate, first ammonium carbonate is dissolved in water to prepare 40 % solution (add 1.5 times the mass of water), and then add it dropwise to diethylenetriaminepentamethylenephosphonic acid under stirring, control the reaction temperature at 80-90°C, raise the temperature to 110-120°C after the addition and continue stirring React for 1.5 hours, evaporate most of the water in the reaction mixture, cool and crystallize, filter, wash, and use the filtrate recovery sleeve to prepare ammonium carbonate solution. The filt...
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