A kind of self-extinguishing waterborne polyurethane resin, preparation method and application
A water-based polyurethane, self-extinction technology, applied in polyurea/polyurethane coatings, coatings, etc., can solve the problems of self-extinction, inability to obtain large molecular chains, small molecular weight, etc., to improve chemical resistance and scratch resistance Non-toxic, easy to handle, and the effect of improving adhesion
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Embodiment 1
[0097] Preparative Example 1: Preparation of 1,3-bis((trimethylol)methylamino)propane
[0098] Mix 1,3-dibromopropane and tris(hydroxymethylaminomethane) in an ethanol solvent with a molar ratio of 1:4, react under reflux conditions for 8 hours, cryogenic crystallisation at -5°C after the reaction, filter and add the filtrate to acidify with HBr To pH 2, then cryogenically crystallized at -5 °C and then suction filtered, the filter cake was taken and dissolved in absolute ethanol, and the pH was adjusted to 10 with sodium hydroxide solution, and then -5 °C cryogenic crystallization, suction filtration, and drying to obtain the product Crude. The crude product was first dissolved in hot absolute ethanol, cooled naturally for 30 min, vacuum filtration to remove insolubles, then recrystallized at room temperature, and filtered to obtain the pure product.
[0099] The NMR characterization is as follows:
[0100] 1 H NMR (CDCl 3 ,400MHz,TMS):δ1.58(m,2H),2.55(t,4H),3.38(m,12H). ...
Embodiment 2
[0101] Preparative Example 2: Preparation of 1,4-bis((trimethylol)methylamino)butane
[0102] 1,4-bis((trimethylol)methylamino)butane was prepared according to the above method, except that the raw material 1,3-dibromopropane was replaced with 1,4-dibromobutane.
[0103] The NMR characterization is as follows:
[0104] 1 H NMR (CDCl 3 ,400MHz,TMS):δ1.4(m,4H),2.45(m,4H),3.48(m,12H).
Embodiment 3
[0105] Preparative Example 3: Preparation of 1,5-bis((trimethylol)methylamino)pentane
[0106] 1,5-bis((trimethylol)methylamino)pentane was prepared according to the above method, except that the raw material 1,3-dibromopropane was replaced with 1,5-dibromopentane.
[0107] The NMR characterization is as follows:
[0108] 1 H NMR (CDCl 3 ,400MHz,TMS):δ1.19(m,2H),1.48(m,4H),2.55(t,4H),3.48(m,12H).
[0109] Example 1
[0110]120 grams of polycaprolactone diol, 2 grams of polyethylene glycol monomethyl ether, 3 grams of dimethylolpropionic acid, and 17.5 grams of 1,4-cyclohexanedimethanol were added to a mixture with a condenser and a stirrer. Add 72 grams of IPDI, 0.08 grams of Bi@8108, and 50 grams of acetone to the four-necked flask of acetone, then add 1.9 grams of dimethylethanolamine, react at 35 degrees for 10 minutes, then add a mixed solution of 9 grams of 1,3-bis((trimethylol)methylamino)propane and 36 grams of deionized water, React at 45 degrees for 30 minutes; ...
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