Flame-retardant waterborne polyurethane emulsion
A water-based polyurethane and emulsion technology, which is applied in the fields of organic chemistry, compounds of Group 5/15 elements of the periodic table, chemical instruments and methods, etc., can solve the problem of water-based polyurethane being easy to burn, and achieve enhanced thermal stability and flame retardant effect. Significant, environmentally friendly effects
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[0026] The preparation method of flame-retardant aqueous polyurethane emulsion of the present invention comprises the steps:
[0027] (1), first dehydrating and drying the polyester diol and the anionic chain extender in a vacuum oven at 60-80° C. for 12 hours to obtain the dried polyester diol and the dried anionic chain extender for subsequent use;
[0028] (2) Add the weighed dry polyester diol, diisocyanate and a small amount of catalyst into a three-necked flask equipped with a stirring device for mixing, feed nitrogen, and heat to 90-100°C for 3-5 hours to obtain polyurethane Prepolymer;
[0029] (3) Add a dry anionic chain extender to the polyurethane prepolymer and react at 85° C. for 1-2 hours to obtain an anionic end-NCO prepolymer;
[0030] (4) Cool down the anionic terminal-NCO prepolymer to 40°C, add a neutralizer dropwise into the system for neutralization reaction for 30-40 minutes, if the viscosity of the system is too high during the cooling period, add an ap...
Embodiment 1
[0047] The preparation method of the flame-retardant aqueous polyurethane emulsion of the present embodiment may further comprise the steps:
[0048] (1), preparation of flame retardant (HCCP-6):
[0049] (1-1), 2,2'-diphenol (4.29g, 23.01mmol) was dissolved in anhydrous tetrahydrofuran (35ml), under N 2 Slowly added dropwise to the solution containing HCCP (4.00g, 11.51mmol), K 2 CO 3 (6.36g, 46.02mmol) and anhydrous tetrahydrofuran solution (30ml) in a three-necked flask; react in ice bath for 30min, then continue to stir the reaction at room temperature. Phosphorus spectrum (31P NMR) was used to track and monitor during the experiment until the phosphorous spectrum signal peak (ζ=20.43pm) of HCCP disappeared. After the reaction, remove the precipitated salts (K 2 CO 3 ), the supernatant was concentrated by rotary evaporation to obtain a crude product; the crude product was recrystallized by a dual-solvent method (dichloromethane:petroleum ether=1:1.5(v:v)), and finally...
Embodiment 2
[0059] The preparation method of the flame-retardant aqueous polyurethane emulsion of the present embodiment may further comprise the steps:
[0060] (1), the preparation steps of flame retardant (HCCP-6) are with embodiment 1.
[0061] (2) Preparation of water-based flame retardant polyurethane emulsion:
[0062] (2-1), first, dehydrate and dry PCL-2000 and DMBA in a vacuum oven at 80°C for 12 hours to obtain dried PCL-2000 and dried DMBA for later use;
[0063] (2-2) Add 57.00g of dry PCL-2000, 22.23g of IPDI and 0.3g of DBTDL into a three-necked flask equipped with a stirring device, feed in nitrogen, and heat to 90°C for 3 hours to obtain a polyurethane prepolymer;
[0064] (2-3) Add 4.17g of dry DMBA to the polyurethane prepolymer and react at 85°C for 2 hours to obtain an anionic end-NCO prepolymer;
[0065] (2-4) Lower the temperature from 85°C to 40°C, add 2.84gTEA dropwise to the anionic end-NCO prepolymer system for neutralization reaction for 30min, if the viscosi...
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