Method for preparing amine-terminated polyether by leaving group method
A technology of amino-terminated polyether and leaving group method, which is applied in the field of preparing amino-terminated polyether by leaving group method, and achieves the effects of good reaction selectivity, less by-products and mild reaction conditions
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example 1
[0043]Example 1: Add the mixed solution of 48.2g (0.30mol) cyclohexyl chloroformate and 50 gram toluene in the four-necked flask that agitator, nitrogen inlet, thermometer and reflux device are equipped, feed nitrogen, 200.0g (0.10 mol) functionality of 2, polyethylene oxide polyol with a molecular weight of 2000 and 23.7g (0.30mol) pyridine mixed solution was added dropwise, the temperature of the reaction system was controlled not to exceed 20°C, and the reaction solution was heated to 40°C after dropping , reacted for 2 hours, and vacuum filtered to obtain a cyclohexyl carbonate-terminated polyether solution containing toluene; then, drop the cyclohexyl carbonate-terminated polyether into 30 g (0.50 mol) of ethylenediamine, and stir at room temperature for 30 min. Then pass the reaction solution through a molecular still (German UIC KDL5 series) at a distillation temperature of 130 ° C and a pressure of 10 Pa to remove excess ethylenediamine, toluene and cyclohexanol produce...
example 2
[0044] Example 2: Add 39.0g (0.24mol) cyclohexyl chloroformate and 50g xylene in a four-necked flask equipped with stirrer, nitrogen inlet, thermometer and reflux device, feed nitrogen, and 200.0g (0.10 mol) functionality of 2, polyethylene oxide polyol with a molecular weight of 2000 and 19.0g (0.24mol) of pyridine was added dropwise, and the temperature of the reaction system was controlled not to exceed 20°C. After the drop, the reaction solution was heated to 50°C ℃, reacted for 2 hours, and vacuum filtered to obtain a cyclohexyl carbonate-terminated polyether solution containing xylene; then drop the cyclohexyl carbonate-terminated polyether into 22.2g (0.30mol) of 1,3-propylenediamine , and stirred at room temperature for 30 minutes. Then pass the reaction solution through a molecular still (German UIC KDL5 series) at a distillation temperature of 130°C and a pressure of 10 Pa to remove excess 1,3-propylenediamine, toluene and cyclohexanol produced by the reaction to obt...
example 3
[0045] Example 3: Add 48.2g (0.30mol) mixed solution of cyclohexyl chloroformate and 100g diethyl carbonate in a four-necked flask equipped with stirrer, nitrogen inlet, thermometer and reflux device, feed nitrogen into 200.0g (0.067mol) a mixed solution of polypropylene oxide polyol with a functionality of 3 and a molecular weight of 3000 and 30.3g (0.30mol) of triethylamine is added dropwise, and the temperature of the reaction system is controlled not to exceed 20°C. After the drop is completed, the reaction solution is heated to 50°C, react for 2 hours, and vacuum filter to obtain a cyclohexyl carbonate-terminated polyether solution containing diethyl carbonate; then drop the cyclohexyl carbonate-terminated polyether into 27.2g (0.20mol) m-phthalylene In the amine, stir at room temperature for 30 min. Then pass the reaction solution through a molecular still (German UIC KDL5 series) at a distillation temperature of 150 °C and a pressure of 1.0 Pa to remove excess m-xylylen...
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