Method of preparing polycarbonate dihydric alcohol
A technology of polycarbonate diol and polycarbonate diol, which is applied in the field of preparation of polycarbonate diol, and can solve problems such as difficult removal and difficult control of the process
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Embodiment 1
[0020] A) In a 1L glass flask, add 427g of diethyl carbonate, 625g of 1,6-hexanediol and 0.084g of tetraisopropyl phthalate, stir and react at 200°C for 3 hours, then stir at 100mmHg Under the pressure, after continuing to react for 5.5 hours, obtain polycarbonate diol 537g containing transesterification catalyst.
[0021] B) Take 100g of the above product in a 500mL reaction flask, add 3g of water at 120°C, stir for 1 hour to deactivate the catalyst, remove excess water under reduced pressure, and obtain polycarbonate without transesterification catalyst Ester diol.
[0022] Polyurethane reaction:
[0023] Add 100 g of the above-mentioned polycarbonate diol that has undergone deactivation treatment into a 500 mL reaction flask, heat it to 70 ° C, then add MDI, take a sample after reacting for 1 hour, and measure the conversion rate of MDI in the system. The results are shown in Table 1 .
Embodiment 2
[0025] 100 g of polycarbonate diol containing transesterification catalyst synthesized by the method in Example 1, added 8.78 mg of tributyl phosphite, heated to 120° C. under continuous stirring, heated and stirred at this temperature for 3 hours, cooled and discharged . Carry out polyurethane reaction with the method of embodiment 1, take a sample after 1 hour, measure the conversion rate of MDI in the system, the results are shown in Table 1.
Embodiment 3
[0027] A) In a 1L glass flask, add 490 g of 1,5-pentanediol, 410 g of diethyl carbonate, 0.08 g of tetraisopropyl phthalate as a transesterification catalyst, stir and react for 4 hours at 150° C., and then Under the pressure of 100 mmHg, after continuing to react for 5.5 hours, the polycarbonate diol containing the transesterification reaction catalyst was obtained.
[0028] B) Take 100g of the above product in a 500mL reaction flask, add 3g of water at 120°C, stir for 1 hour to deactivate the catalyst, remove excess water under reduced pressure, and obtain polycarbonate without transesterification catalyst Ester diol.
[0029] Polyurethane reaction:
[0030] Add 100 g of the above-mentioned polycarbonate diol that has undergone deactivation treatment into a 500 mL reaction flask, heat it to 70 ° C, then add MDI, take a sample after reacting for 1 hour, and measure the conversion rate of MDI in the system. The results are shown in Table 1 .
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