Method for synthesizing carvacrol with epoxy limonene foot oil
A technology of epoxy limonene and carvacrol, which is applied in the chemical industry, can solve problems such as limited application, environmental pollution, aluminum salt and iron salt solid waste, and achieve the effect of solving environmental protection problems
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Embodiment 1
[0020] Step 1: Add 500g of epoxy limonene foot oil (60% diethylene glycol content, 300g), 300g of toluene and 15g of p-toluenesulfonic acid into a 1000 mL reactor, then react at 120-150°C for about 3-4 hours, GC After showing that the reaction is over, lower the temperature of the kettle to below 40°C and add 250g of 5wt% NaHCO 3 The aqueous solution was washed to pH=7-8, and the organic phase obtained by liquid separation was rectified under reduced pressure to obtain 230 g of isodihydrocarvone with a content greater than 90%, with a yield of 86%.
[0021] Step 2 Put 230g of isodihydrocarvone and 20g of xylene obtained above into a 500 mL three-neck flask, then add 180g of catalyst B, and react under reflux at 190-220°C. During the reaction, pump the reaction liquid continuously Blow air under the face, about 4-5 hours, GC shows that 40% of isodihydrocarvone remains, stop the reaction, filter to remove the catalyst, carry out vacuum distillation on the filtrate, recover 14g o...
Embodiment 2
[0024] Step 1: Add 500g of epoxy limonene foot oil (60% diethylene glycol content), 300g of toluene and 10g of p-toluenesulfonic acid into a 1000 mL reactor, then react at 120-150°C for about 4-5 hours, GC shows that the reaction After the end, reduce the kettle temperature to below 40°C, add 200g 5wt% NaHCO 3 The aqueous solution was washed to PH = 7-8, and the organic phase obtained by liquid separation was rectified under reduced pressure to obtain 225 g of isodihydrocarvone with a content greater than 90%, with a yield of 84%.
[0025] Step 2 Put 225g of isodihydrocarvone and 20g of xylene obtained above into a 500 mL three-necked flask, then add 115g of catalyst B, and react under reflux at 190-220°C. During the reaction, pump continuously to the reaction solution Blow air under the face, about 5-6 hours, GC shows that 38% of isodihydrocarvone remains, stop the reaction, filter to remove the catalyst, carry out vacuum distillation on the filtrate, recover 15g of solvent a...
Embodiment 3
[0027] Step 1: Add 500g of epoxy limonene foot oil (60% diethylene glycol content), 300g of toluene and 5g of p-toluenesulfonic acid into a 1000 mL reactor, then react at 120-150°C for 6-7 hours, GC shows that the reaction is complete After that, the temperature of the kettle was lowered to below 40°C, and 170g of 5wt% NaHCO was added 3 The aqueous solution was washed to PH = 7-8, and the organic phase obtained by liquid separation was rectified under reduced pressure to obtain 213 g of isodihydrocarvone with a content greater than 90%, with a yield of 80%.
[0028] Step 2 Put 213g of isodihydrocarvone and 20g of xylene obtained above into a 500 mL three-necked flask, then add 50g of catalyst B, and react under reflux at 190-220°C. During the reaction, pump continuously to the reaction solution Blow air under the face, about 9 to 10 hours, GC shows that 33% of isodihydrocarvone remains, stop the reaction, remove the catalyst by filtration, carry out vacuum distillation on the ...
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