反应详情

温度

105 °C

A 250 ml flask with stir bar was charged with: 57 g of bisphenol-A (0.25 mole=0.50 equivalents) and 56 g (65 ml) of xylene. This was heated to 105° C. and there was then added 0.5 g of 50% triflic acid in water. Then 41 ml (34.4 g) d-limonene (99%) was added over 25 minutes at 105° C.±2° C. The reaction temperature was allowed to drop to 90° C. over 35 minutes at which time it was raised to 105° C. and an additional 40 ml of d-limonene (total of 68 g, 0.5 mols) was added over 45 minutes. After 1.5 hours at 105° C. catalyst was neutralized with 0.5 g of 15% sodium hydroxide in water. The well stirred reaction mixture was then allowed to stand overnite at room temperature. Then 176 g of liquor was separated from solid (salt), xylene, and unreacted d-limonene removed by vacuum distillation to 166° C. at 30 inches of vacuum. Yield of product and distillate was 111 g and 63 g respectively. Product was characterized by 3.8% free bisphenol-A; Mw/Mn of 310/235; and viscosity of 1250 cps (100° C.).

1. temperaturewas raised to 105° C.
2. stirringThe well stirred
3. customreaction mixture
4. customto stand overnite at room temperature
5. customThen 176 g of liquor was separated from solid (salt), xylene, and unreacted d-limonene
6. customremoved by vacuum distillation to 166° C. at 30 inches of vacuum
7. customviscosity of 1250 cps (100° C.)