Radical polymerizable polyether, method for producing same, polymerizable composition, copolymer, molded article and film
A technology of a polymeric composition and a manufacturing method, applied in the fields of free radically polymerizable polyether and its manufacture, polymeric composition, copolymer, molded body, and film, capable of solving undisclosed problems
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[0106] Hereinafter, the present invention will be specifically described with reference to examples.
[0107] The evaluation of the radical polymerizable polyether (A) was implemented by the following method.
[0108] (1) 1 H-NMR spectrum
[0109] pass 1 H-NMR spectrum confirmed the structure of the compound.
[0110] CDCl3 was used as a measurement solvent, tetramethylsilane was used as a reference substance, and measurement was performed using a nuclear magnetic resonance apparatus (JNM EX-270: manufactured by JEOL Ltd.). The measurement was performed under the conditions that the measurement temperature was room temperature and the number of accumulations was 16 times.
[0111] (2) Molecular weight determination
[0112] Based on polystyrene, the number average molecular weight of the polymer by GPC (HLC-8220: manufactured by Tosoh Co., Ltd., column: TSK-GEL SUPER H-4000 and TSK-GEL SUPER H-2000 connected in series) (Mn), mass average molecular weight (Mw) and molecul...
manufacture example 1
[0130] 600 g of tetrahydrofuran (manufactured by Wako Pure Chemical Industries, Ltd.) and 2 g of ytterbium (III) trifluoromethanesulfonate hydrate (manufactured by Tokyo Chemical Industry Co., Ltd.) were added to a 1000 ml three-necked flask equipped with a stirring bar, a thermometer, and a cooling tube. Stirring was carried out at room temperature. After confirming that the ytterbium trifluoromethanesulfonate hydrate was dissolved, 24 g of glycidyl methacrylate (manufactured by Wako Pure Chemical Industries, Ltd.) was added. After the addition, it was stirred at room temperature (25° C.) for 11 hours. After stirring, 50 g of ethanol (manufactured by Wako Pure Chemical Industries, Ltd.) was added to stop the reaction. After completion of the reaction, unreacted tetrahydrofuran and excess ethanol were distilled off using an evaporator to obtain 437 g of a white solid (yield 70%).
[0131] The obtained white solid had a mass average molecular weight of 45,000 as measured by G...
manufacture example 2
[0135] Production Example 1 was carried out in the same manner as in Production Example 1, except that the usage amounts and reaction time of tetrahydrofuran, glycidyl methacrylate, ytterbium trifluoromethanesulfonate hydrate, and ethanol were changed to those shown in Table 1. As measured by GPC, the mass average molecular weight was 14500. In addition, when the degree of polymerization of the skeleton derived from glycidyl methacrylate is represented by m and the degree of polymerization of tetrahydrofuran is represented by n, the introduction rate of the skeleton derived from glycidyl methacrylate m1 / (m1+m2+n ) is 0.081.
[0136] [Manufacturing example 1']
[0137] 60 g of the whitened solid obtained in Production Example 1 was transferred to a separating funnel, and 90 ml of ethyl acetate and 90 ml of pure water were added to perform a liquid separation operation. The washed organic layer was dehydrated using anhydrous magnesium sulfate. After filtering this, ethyl acet...
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Abstract
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