Water-dispersible polyisocyanate cross-linking agent and preparation method thereof
A polyisocyanate and crosslinking agent technology, applied in polyurea/polyurethane coatings, coatings, etc., can solve the problems of long drying time, high polyether content and high price
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Embodiment 1
[0046]
[0047] In a 250 ml three-necked round-bottomed flask equipped with a thermometer and a stirrer, 100 grams of compound VI (PEG-200, with an average molecular weight of 190-210) and 75 grams of triethylamine were added under nitrogen protection; Add 76 g of O, O-dimethoxyphosphoryl chloride, and stir the reaction at room temperature after the dropwise addition. Samples were taken during the reaction and monitored by LC-MS until compound VI disappeared, washed with a small amount of water and dried in a vacuum oven to obtain compound VII. The compound was characterized by proton nuclear magnetic resonance, and a characteristic triplet peak at about 4.2ppm was seen.
Embodiment 2
[0049] Add 100 grams of compound VI (PEG-200, with an average molecular weight of 190-210) and 75 grams of triethylamine in a 500 ml three-necked round-bottomed flask equipped with a thermometer, a stirrer and a reflux condenser; slowly dropwise add O,O-dimethoxyphosphoryl chloride (solution of 76 g in 50 ml of toluene). During the reaction, samples were taken and LC-MS was used to monitor the reaction until compound VI disappeared. The above reaction liquid was distilled off the solvent under reduced pressure, washed with water and dried in a vacuum oven to obtain compound VII.
Embodiment 3
[0051] Add 1 kg of compound VI (PEG-200, with an average molecular weight of 190-210) and 0.75 kg of triethylamine into a 10-liter reactor equipped with a thermometer, a stirrer and a reflux condenser. The above mixture was cooled to 0°C, and 0.76 kg of O,O-dimethoxyphosphoryl chloride was slowly added dropwise, and the temperature was controlled below 10°C during the dropwise addition; after the drop was completed, the temperature was raised to room temperature for reaction. Samples were taken during the reaction and the reaction was monitored by LC-MS until compound VI disappeared. Compound VII was obtained by separating by beating with water and drying in a vacuum oven.
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