A kind of organosilicon borate modified ammonium polyphosphate and its preparation method and application
A technology of borosilicate and ammonium polyphosphate, which is applied in the direction of flame-retardant fibers, textiles, papermaking, fiber treatment, etc., can solve problems such as moisture return, easy moisture absorption, and decreased flame-retardant performance, so as to improve hygroscopicity and increase additional value, the effect of improving flame retardancy
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Embodiment 1
[0029] (1) Silicone borate
[0030] Mix 0.1mol n-dodecane bromide, 0.105mol diethanolamine, 50mL dimethylformamide and 10.6g Na 2 CO 3 Place in a 250mL four-neck flask equipped with an electric stirring device and a condenser, control the constant temperature water bath at 90°C, stir and react for 6h, cool slightly, filter to remove residual solids in the solution, and distill the mother liquor under reduced pressure at 170°C to remove unreacted raw materials and solvents to obtain the product N, N-dihydroxyethyl dodecylamine.
[0031] Add 0.02mol N,N-dihydroxyethyldodecylamine, 0.02mol triethyl borate and 40mL benzene into a 100mL four-necked flask equipped with an electric stirring device, an oil-water separator and a vacuum decompression device. The oil-water separator is pre-loaded with zinc chloride solid to remove the ethanol generated by the reaction by reflux under reduced pressure. The temperature of the water bath is 60°C, and the vacuum degree is controlled to 0....
Embodiment 2
[0038] (1) Silicone borate
[0039] Mix 0.1mol n-dodecane bromide, 0.105mol diethanolamine, 50mL dimethylformamide and 10.6g Na 2 CO 3 Place in a 250mL four-neck flask equipped with an electric stirring device and a condenser, control the constant temperature water bath at 90°C, stir and react for 6h, cool slightly, filter to remove residual solids in the solution, and distill the mother liquor under reduced pressure at 170°C to remove unreacted raw materials and solvents to obtain the product N,N-Dihydroxyethyl dodecylamine.
[0040] Add 0.02mol N,N-dihydroxyethyldodecylamine, 0.02mol triethyl borate and 40mL benzene into a 100mL four-necked flask equipped with an electric stirring device, an oil-water separator and a vacuum decompression device. The oil-water separator is pre-loaded with zinc chloride solid to remove the ethanol generated by the reaction by reflux under reduced pressure. The water bath temperature is 60°C, and the vacuum degree is controlled to 0.04Mpa to...
Embodiment 3
[0047] (1) Silicone borate
[0048] Mix 0.1mol n-dodecane bromide, 0.105mol diethanolamine, 50mL dimethylformamide and 10.6g Na 2 CO 3 Place in a 250mL four-neck flask equipped with an electric stirring device and a condenser, control the constant temperature water bath at 90°C, stir for 6 hours, cool slightly, filter to remove residual solids in the solution, and distill the mother liquor under reduced pressure at 170°C to remove unreacted raw materials and solvents to obtain the product N, N-dihydroxyethyl dodecylamine.
[0049] Add 0.02mol N,N-dihydroxyethyldodecylamine, 0.02mol triethyl borate and 40mL benzene into a 100mL four-necked flask equipped with an electric stirring device, an oil-water separator and a vacuum decompression device. The oil-water separator is pre-loaded with zinc chloride solid to remove the ethanol generated by the reaction by reflux under reduced pressure. The temperature of the water bath is 60°C, and the vacuum degree is controlled to 0.04Mpa...
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