Process for production of polycarbonate diol diacrylate and high-purity polycarbonate diol diacrylate
A technology of polycarbonate diol diacrylate and polycarbonate diol, which is applied in the field of high-purity polycarbonate diol diacrylate, can solve problems such as ignorance, and achieve bridging density without reducing and inhibiting Excellent effect of exchange reaction, efficiency and safety
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Embodiment 1
[0125] Acrylation of embodiment 1 polycarbonate diol
[0126] Add 5 mmol of vinyl acrylate to 1.0 g (0.5 mmol) of polycarbonate diol (UH200 manufactured by Ube Industries, (poly(hexamethylene carbonate)) diol: average molecular weight 2000 (polymerization degree 14.6)) and Toluene was added to 1 mg of p-methoxyphenol as a polymerization inhibitor, and the volume was fixed to 10 ml to prepare a reaction solution.
[0127] 2 ml of the above reaction solution and 20 mg of lipase immobilized in a resin porous body (Novozyme 435 (manufactured by Novozymes Co., Ltd.) derived from Candida antarctica (Candida antarctica) lipase) were added to a glass test tube, and stirred (1000 rpm) , and reacted at 70° C. for 24 hours.
[0128] After the reaction, the reaction solution was filtered with a filter with a pore size of 0.2 μm, and the solvent was distilled off from the filtrate under reduced pressure with a rotary evaporator, and the residue was dried in a desiccator at 60° C. under r...
Embodiment 5～7
[0136] Acrylation of embodiment 5~7 polycarbonate diol
[0137] To 3.0 g of polycarbonate diol shown in Table 2, vinyl methacrylate (1.35 g in Example 5 (UH100) and 1.35 g in Example 6 (UC100) and Example 7 (1.51 g in UM90 (1 / 1): polycarbonate diol with equimolar residues of 1,6-hexanediol and 1,4-cyclohexanedimethanol)) and as a polymerization inhibitor Toluene was added to 1 mg of p-methoxyphenol as the solvent, and the volume was fixed to 10 ml to prepare a reaction solution.
[0138] 2 ml of each reaction solution and 5 mg of lipase (Novozyme 435) were added to a glass test tube, and reacted for the time shown in Table 2 at 70° C. under stirring (1000 rpm).
[0139] After the completion of the reaction, each reaction liquid was filtered with a 0.2 μm filter, and the solvent was distilled off under reduced pressure with a rotary evaporator for each filtrate, and each residue was dried in a desiccator at 60° C. under reduced pressure for 2 hours to obtain each polycarbona...
Embodiment 8～10
[0145] Examples 8-10: Propylene based on polycarbonate diol for continuous reaction using immobilized enzyme Esterification
[0146] Add 67.5g of vinyl methacrylate and 0.05g of p-methoxyphenol as a polymerization inhibitor to 150g of polycarbonate diol (UH100, refer to Table 2), add toluene to it, and after the volume is set to 500ml, it is prepared The reaction solution.
[0147] 0.42 g of immobilized lipase (Novozyme 435) was filled in a glass column (a glass filter with an inner diameter of 5 mm × 50 mm and a pore size of 5 μm), kept at 70° C., and the reaction solution was delivered from below at the flow rate shown in Table 4 by a quantitative pump.
[0148] The reaction solution was fractionated according to the time shown in Table 4, and the solvent was distilled off the obtained reaction solution under reduced pressure with a rotary evaporator, and the residue was dried in a desiccator at 60° C. under reduced pressure for 2 hours, and supplied to 1 H-NMR analysis...
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