Curable composition and cured product from same
一种固化性组合物、化合物的技术,应用在其他家里用具、应用、仪器等方向,能够解决成本增多、无法得到高精度固化物等问题
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preparation example 1
[0227] [Preparation Example 1: Synthesis of (3,4,3',4'-diepoxy)bicyclohexane (a-1)]
[0228] 70 g (0.68 mol) of 95% by weight sulfuric acid and 55 g (0.36 mol) of 1,8-diazabicyclo[5.4.0]undecene-7 (DBU) were stirred and mixed to prepare a dehydration catalyst.
[0229] Into a 3L flask equipped with a stirrer, a thermometer, and a distillation pipe filled with a dehydrating agent and insulated, 1000 g (5.05 moles) of hydrogenated biphenol (4,4'-dihydroxybicyclohexane), the above-mentioned 125 g of the prepared dehydration catalyst (0.68 mol as sulfuric acid) and 1500 g of trimethylene were heated in the flask. Formation of water was confirmed when the internal temperature exceeded 115°C. Furthermore, heating was continued until the temperature reached the boiling point of mesitylene (internal temperature: 162 to 170° C.), and a dehydration reaction was carried out under normal pressure. By-product water is distilled and discharged out of the system through the dehydration pip...
preparation example 2
[0234] [Preparation Example 2: Synthesis of bis(3,4-epoxycyclohexylmethyl) ether (a-2)]
[0235] 499 g (12.48 mol) of sodium hydroxide (granular form) and 727 mL of toluene were added to a 5 L reactor, and after nitrogen substitution, 484 mL of a toluene solution of 420 g (3.74 mol) of tetrahydrobenzyl alcohol was added and aged at 70° C. for 1.5 hours. Then, tetrahydrobenzyl methanesulfonate (419 g, 2.20 mol) was added, it refluxed for 3 hours, it aged, it cooled to room temperature, and water (1248g) was added to stop reaction, and liquid-separated.
[0236] The organic layer obtained by liquid separation was concentrated, and distilled under reduced pressure to obtain bis(tetrahydrobenzyl)ether (yield: 85%) as a colorless transparent liquid. The obtained bis(tetrahydrobenzyl) ether was measured 1 H-NMR spectrum.
[0237] 1 H-NMR (CDCl 3 ): δ1.23-1.33(m, 2H), 1.68-1.94(m, 6H), 2.02-2.15(m, 6H), 3.26-3.34(m, 4H), 5.63-7.70(m, 4H)
[0238] 200 g (0.97 mol) of the obtained...
Embodiment 1~6
[0239] Examples 1-6, and comparative examples 1-3
[0240] Each component was mixed according to the recipe (unit: part by weight) described in following Table 1, and the curable composition was obtained.
[0241] [Calculation method of SP value]
[0242] The SP value (solubility parameter: δ) of each compound in Table 1 is a value at 25°C based on Fedors' method. Calculated based on the method described in Polym. Eng. Sci., 14, 147 (1974). Specifically, it is calculated according to the following formula. In addition, the evaporation energy and molar volume of an atom or an atomic group employ|adopted the well-known value using the said document etc..
[0243] δ=(Σei / Σvi) 1 / 2
[0244] ei: Evaporation energy of an atom or group of atoms
[0245] vi: Molar volume of an atom or group of atoms
[0246] [Calculation method of average SP value]
[0247] The curable composition contains n curable compounds, and the SP values of the curable compounds are respectively x 1 、...
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