Polycarbonate diol and preparation method thereof
A polycarbonate diol and carbonate technology, applied in the directions of products, educts, reagents, etc., can solve the problems of low sales volume, difficult to precisely control the molecular weight of polycarbonate diols, and few fields, so as to increase the molecular weight and broaden the application. , the effect of reducing waste
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[0045] And the invention provides a kind of preparation method of polycarbonate diol.
[0046] The technical solution is:
[0047] A preparation method of polycarbonate glycol, comprising the following steps:
[0048] Using polyols and carbonates as main raw materials, the crude product of polycarbonate diols is prepared through transesterification and polycondensation;
[0049] Collect the polycarbonate diol crude product with molecular weight at 600~1100;
[0050] Mix the crude polycarbonate diol with a molecular weight of 600-1100, an organic dibasic acid and a dehydrating agent, stir for reaction, and suction filter to prepare the polycarbonate diol.
[0051] In the process of preparing polycarbonate diols by transesterification, the present invention collects crude polycarbonate diols with lower molecular weight (600-1100), and expands them by adding organic dibasic acids and dehydrating agents. chain, increase the molecular weight, and at the same time, it can also ensu...
Embodiment 1
[0088] The present embodiment provides a kind of polycarbonate diol and preparation method thereof, and the steps are as follows:
[0089] step 1)
[0090] Set the initial temperature of the reactor to 95°C, and the pressure in the reactor to normal pressure. In terms of the amount of substances, 100 parts of 1,4-butanediol, dimethyl carbonate, and 120 parts and 1.5 parts of catalyst sodium methylate, then increase the temperature in the reactor isocratically, to a temperature of 160°C, and carry out atmospheric distillation reaction (i.e. the first stage reaction) for 6.5h; after the above reaction is completed, the reactor The negative pressure of the internal system was reduced to 100Pa-10000Pa, and then the temperature was kept at 160°C. Under this pressure and temperature, the reaction was distilled under reduced pressure (ie, the second-stage reaction) for 7.5 hours to complete the transesterification polycondensation reaction and obtain the product intermediate.
[009...
Embodiment 2
[0098] The present embodiment provides a kind of polycarbonate diol and preparation method thereof, and concrete steps are as follows:
[0099] step 1)
[0100] Set the initial temperature of the reactor to 95°C, and the pressure inside the reactor to normal pressure. In terms of the amount of substances, 100 parts of 1,6-hexanediol, dimethyl carbonate, and 120 parts and 1.5 parts of catalyst sodium methylate, then increase the temperature in the reactor isocratically, to a temperature of 160°C, and carry out atmospheric distillation reaction (i.e. the first stage reaction) for 6.5h; after the above reaction is completed, the reactor The negative pressure of the system was reduced to 100Pa~10000Pa, and then the temperature was kept at 160°C. Under the pressure and temperature, the vacuum distillation reaction (that is, the second stage reaction) was carried out for 8.5 hours to complete the transesterification polycondensation reaction and obtain the product intermediate.
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