Method for preparing carvacrol by recycling carvone synthesis by-product
A technology for carvacrol and carvone is applied in the field of recovering by-products from synthesizing carvone to prepare carvacrol, which can solve the problems of environmental protection, high separation difficulty, waste and the like, and achieves convenient operation, good quality and high product quality. high yield effect
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Embodiment 1
[0015] Under the protection of nitrogen, add 100 grams of fractions with a mass content of 83.2% of carvacrol into a 500ml flask, add 280 grams of 15% sodium hydroxide solution dropwise under stirring and cooling in a water bath, maintain the temperature at 33°C, and drop for about 4 hours. After the addition, continue to react for half an hour, stand and separate layers; the organic phase is washed with saturated brine and rectified to obtain 13 grams of carvone; the aqueous phase is under nitrogen protection, stirring and ice-water bath, and 10% hydrochloric acid with a mass concentration of 10% is added dropwise The pH value of the solution was adjusted to 5.0, the titration rate was controlled, the temperature was maintained at 25° C., the layers were left to stand, the organic phase was washed with saturated saline solution, and 80.4 g of carvacrol was obtained by rectification under reduced pressure, with a content of 99.35% and a yield of 96.6%.
Embodiment 2
[0017] Under the protection of nitrogen, add 100 grams of fractions with a mass content of 86.2% carvacrol into a 500ml flask, add 250 grams of 15% sodium hydroxide solution dropwise under stirring and cooling in a water bath, maintain the temperature at 35°C, and drop for about 4.5 hours After the addition, continue to react for half an hour, let stand and separate layers; the organic phase is washed with saturated brine, and rectified to obtain 12 grams of carvone; The pH value was 6.0, the titration rate was controlled, the temperature was maintained at 20°C, the layers were allowed to stand, the organic phase was washed with saturated saline solution, and 82.7 g of carvacrol was obtained by rectification under reduced pressure, with a content of 99.45% and a yield of 95.9%.
Embodiment 3
[0019] Under the protection of nitrogen, add 100 grams of fractions with a mass content of 85.7% carvacrol into a 500ml flask, add 280 grams of potassium hydroxide solution with a mass concentration of 17% under stirring and cooling in a water bath, and keep the temperature at 32°C for about 5 hours. After the addition, continue to react for half an hour, stand and separate layers; the organic phase is washed with saturated brine, and rectified to obtain 12.3 g of carvone; the aqueous phase is under nitrogen protection, stirring and ice-water bath, and 10% hydrochloric acid is added dropwise The pH value of the solution was adjusted to 5.5, the titration rate was controlled, the temperature was maintained at 22°C, the layers were allowed to stand, the organic phase was washed with saturated saline solution, and 83.1 g of carvacrol was obtained by rectification under reduced pressure, with a content of 99.43% and a yield of 97%.
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