Method for preparing versatate glycidyl
A technology of glycidyl ester and tertiary carbonic acid is applied in the field of preparation of glycidyl tertiary carbonate, can solve the problems of low yield of glycidyl tertiary carbonate and high preparation cost, and achieves a product with good product quality, low preparation cost and high purity. Effect
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[0037] Example 1: Such as figure 1 As shown, a method for preparing glycidyl tertiary carbonate includes the following steps:
[0038] A. Into a four-necked 1L flask with stirring, thermometer and reflux, add 100g ethanol, 100g water and 69.4g epichlorohydrin, heat to 55℃, add 129.3g tertiary carbonic acid and 12.3g sodium hydroxide solution ( Sodium hydroxide (50% by weight) was added dropwise to the flask, the feeding time was controlled to 20 minutes, and the reaction was carried out at 55°C for 2.0 hours;
[0039] B. Cool the reaction mixture obtained in step A to 40°C, separate the water phase, add 24 g of sodium hydroxide and 74 g of water, and then react at 40°C for 80 minutes;
[0040] C. Distill the reaction mixture obtained in step B at a pressure of 5KPa and a temperature of 120°C, and then add 20mL of water for steam stripping. Keep the pressure at 5KPa and a temperature of 140°C for 10 minutes to remove excess epichlorohydrin. , Solvents and water and chloride salts ge...
Example Embodiment
[0042] Example 2: Such as figure 1 As shown, a method for preparing glycidyl tertiary carbonate includes the following steps:
[0043] A. Into a four-necked 2L flask with stirring, thermometer and reflux, add 400g isopropanol, 605g water and 300g epichlorohydrin, heat to 80℃, add 500g tertiary carbonic acid and 47.6g sodium hydroxide solution ( Sodium hydroxide (50% by weight) was dropped into the flask, the feeding time was controlled to 20 minutes, and the reaction was carried out at 80°C for 100 minutes;
[0044] B. Cool the reaction mixture obtained in step A to 60°C, separate the water phase, add 93 g of sodium hydroxide and 280 g of water, and then react at 60°C for 100 minutes;
[0045] C. Distill the reaction mixture obtained in step B at a pressure of 95.4KPa and a temperature of 120°C, and then continue vacuum distillation until the pressure is 5KPa and a temperature of 140°C. Remove excess epichlorohydrin, solvent and reaction products The water and chloride salt to obta...
Example Embodiment
[0047] Example 3: Such as figure 1 As shown, a method for preparing glycidyl tertiary carbonate includes the following steps:
[0048] A. Add 124.9g tert-butanol, 100g water and 234.9g epichlorohydrin to a four-necked 1L flask with stirring, thermometer and reflux, and heat to 65°C, add 129.3g tertiary carbonic acid and 12.3g hydrogen hydroxide Sodium solution (50% by weight of sodium hydroxide) was dropped into the flask, the feeding time was controlled to 20 minutes, and the reaction was carried out at 65°C for 30 minutes;
[0049] B. Cool the reaction mixture obtained in step A to 55°C, separate the water phase, add 24.0g potassium hydroxide and 74g water, and then react at 55°C for 30 minutes;
[0050] C. Distill the reaction mixture obtained in step B at a pressure of 95.4KPa and a temperature of 120°C, and then continue vacuum distillation until the pressure is 5KPa and a temperature of 140°C. Remove excess epichlorohydrin, solvent and reaction products The water and chloride...
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