Preparation method of dehydroabietic acid
A technology of dehydroabietic acid and abietic acid type, applied in the field of preparation of dehydroabietic acid, can solve the problems of high cost, complicated process, low yield and the like, and achieves improvement of yield, reduction of production cost and usage of solvent reduced effect
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Embodiment 1
[0034] (1) Take 250 grams of masson pine rosin, crush it and put it into a three-necked flask equipped with a reflux device, heat it under nitrogen protection, raise the temperature to 280 ° C for 40 minutes, cool it down to 60 ° C, add a mixture of ethyl acetate and methanol solution 700ml (25°C, the volume ratio of ethyl acetate to methanol is 92:8), heat up to reflux the solution, cool down to 5°C after the rosin is completely dissolved, let it stand for 24 hours, filter out the crystals, and use an oven under the protection of nitrogen for 100 ℃ drying to constant weight, to obtain 177.9 grams of product A, the yield was 71.16%, and the components of resin acid were measured by gas chromatography, as shown in Table 1;
[0035] (2) Weigh 100 grams of product A, weigh 0.045 grams of palladium carbon (5% palladium content) with an analytical balance, put it into a three-necked flask, evacuate the air, inject nitrogen to decompress and maintain a small flow rate, and heat up to...
Embodiment 2
[0037] (1) Take 250 grams of masson pine rosin, crush it and put it into a three-necked flask equipped with a reflux device, heat it under nitrogen protection, raise the temperature to 275 ° C for 60 minutes, cool it down to 60 ° C, add a mixture of ethyl acetate and methanol solution 700ml (25°C, the volume ratio of ethyl acetate to methanol is 92:8), heat up to reflux the solution, cool down to 5°C after the rosin is completely dissolved, let it stand for 24 hours, filter out the crystals, and use an oven under the protection of nitrogen for 100 ℃ drying to constant weight, product A175.5 g was obtained, and the productive rate was 70.2%, and the components of resin acid were measured by gas chromatography, as shown in Table 1;
[0038] (2) Weigh 100 grams of product A, weigh 0.05 grams of palladium carbon (5% palladium content) with an analytical balance, put it into a three-necked flask, evacuate the air, inject nitrogen to decompress and maintain a small flow rate, and hea...
Embodiment 3
[0040] (1) Take 250 grams of masson pine rosin, crush it and put it into a three-necked flask equipped with a reflux device, heat it under nitrogen protection, raise the temperature to 285°C for 30 minutes, cool down to 60°C, add a mixture of ethyl acetate and methanol solution 700ml (25°C, the volume ratio of ethyl acetate to methanol is 92:8), heat up to reflux the solution, cool down to 5°C after the rosin is completely dissolved, let it stand for 24 hours, filter out the crystals, and use an oven under the protection of nitrogen for 100 ℃ drying to constant weight, product A182.1 g was obtained, and the productive rate was 72.84%. The components of resin acid were measured by gas chromatography, as shown in Table 1;
[0041](2) Weigh 100 grams of product A, weigh 0.038 grams of palladium carbon (5% palladium content) with an analytical balance, put it into a three-necked flask, evacuate the air, inject nitrogen to decompress and maintain a small flow rate, and heat up to 29...
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