Polycarbonate diol and polyurethane obtained using polycarbonate diol
A technology of polycarbonate diol and polycarbonate II, which is applied in the field of polyurethane, can solve the problems of hard texture, high soft segment cohesion, poor chemical resistance, etc., and achieve the effect of excellent elastic recovery
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[0494] Examples and comparative examples are given below to describe the present invention more specifically, but the present invention is not limited to these examples unless the gist of the present invention is exceeded.
[0495] Hereinafter, the evaluation method of each physical property value is as follows.
[0496] [Evaluation method: polycarbonate diol]
[0497]
[0498] Dissolve polycarbonate diol in CDCl 3 , measured at 400MHz 1 H-NMR (AL-400 manufactured by JEOL Ltd.) identified phenoxy groups, dihydroxy compounds, and phenols from the signal positions of each component, and calculated their respective contents from integral values. The detection limit at this time is 100 ppm as the weight of phenol with respect to the weight of the whole sample, and 0.1% by weight of dihydroxy compounds such as the compound represented by the above formula (A) and the compound represented by the above formula (B). In addition, the ratio of the phenoxy group was obtained from th...
Embodiment 1-1
[0561]
[0562] In a 5 L glass separable flask equipped with a stirrer, a distillate collector, and a pressure regulator, 1,4-butanediol (1,4BD) was added as a raw material: 768.5 g, 1,10- Decanediol (1,10DD): 768.5 g, diphenyl carbonate: 2563.0 g, magnesium acetate tetrahydrate aqueous solution: 6.6 mL (concentration: 8.4 g / L, magnesium acetate tetrahydrate: 55 mg), and nitrogen replacement was performed. While stirring, the internal temperature was raised to 160°C, and the contents were dissolved by heating. Then, after reducing the pressure to 24 kPa over 2 minutes, it was allowed to react for 90 minutes while removing phenol from the system. Next, the pressure was lowered to 9.3 kPa over 90 minutes, further lowered to 0.7 kPa over 30 minutes to continue the reaction, and then the temperature was raised to 170°C to remove phenol and unreacted dihydroxy compounds from the system, and the reaction was carried out for 60 minutes. A composition containing polycarbonate diol ...
Embodiment 1-2~ Embodiment 1-13
[0572]
[0573] In the manufacture of the polycarbonate diol of Example 1-1, except that the type and feed amount of the PCD polymerization raw material were changed to the type and feed amount of the raw material recorded in Table 1, all were carried out under the same conditions and methods reaction to obtain a polycarbonate-containing composition.
[0574] The obtained polycarbonate diol-containing composition was subjected to thin film distillation in the same manner as in Example 1-1. Table 1 shows the properties and evaluation results of physical properties of the polycarbonate diol obtained by thin film distillation.
[0575]
[0576] In the manufacture of the polyurethane of Example 1-1, except that the type of polycarbonate diol (PCD) used and the feed amount of each raw material were changed to PCD and the feed amount recorded in Table 3, all were carried out in the same manner. The conditions and methods are used to react to obtain a polyurethane solution. The...
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