A method for crystallization and purification of low-concentration eucalyptus oil
A low-concentration eucalyptus oil technology, applied in the direction of organic chemistry, can solve the problems that the total yield is greatly affected by the rectification yield, eucalyptus oil is difficult to produce shaped crystals, and the intermediate process cannot be monitored, so as to avoid Effect of stringent requirements, fewer types of equipment, and shortened temperature range
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Embodiment 1
[0027] Embodiment 1: the method for the crystallization and purification of this low-concentration eucalyptus oil, the specific operations are as follows:
[0028] (1) Place the eucalyptus oil raw material (eucalyptus oil containing 60% by mass percent 1,8-cineole) in a temperature-controlled bath, cool down to -17°C, stabilize for 5 minutes, and add seed crystals (seed crystals are Prepared by freezing 1,8-cineole with a purity of 99.7% at -20°C), after continuing to stabilize for 5 minutes, cool down to -26°C at a cooling rate of 6°C / h, and after stabilizing for 20 minutes, filter and separate Obtain crude crystal and mother liquor, wherein the addition of crystal seed is 0.2% of the eucalyptus oil raw material quality;
[0029] (2) Heating the crude crystals at a heating rate of 3°C / h, collecting the sweat every time the temperature rises by 3°C, raising the temperature to -6°C, separating the sweat, and obtaining a crystallization product with a purity of 88.32% and a yiel...
Embodiment 2
[0031] Embodiment 2: the method for the crystallization and purification of this low-concentration eucalyptus oil, the specific operations are as follows:
[0032] (1) Place the eucalyptus oil raw material (eucalyptus oil containing 55% by mass percent 1,8-cineole) in a temperature-controlled bath, cool down to -18°C, stabilize for 5 minutes, and add seed crystals (seed crystals are Prepared by freezing 1,8-cineole with a purity of 99.7% at -15°C), after continuing to stabilize for 8 minutes, cool down to -25°C at a cooling rate of 4°C / h, and after stabilizing for 25 minutes, filter and separate Obtain crude crystal and mother liquor, wherein the addition of crystal seed is 0.3% of the eucalyptus oil raw material quality;
[0033] (2) The crude crystals were heated at a heating rate of 4°C / h, sweat was collected every 3°C, and the temperature was raised to -7°C to separate the sweat to obtain a primary crystallization product with a purity of 89.63% and a yield of 54.31%. Swe...
Embodiment 3
[0035] Embodiment 3: the method for the crystallization and purification of this low-concentration eucalyptus oil, the specific operations are as follows:
[0036] (1) Place the eucalyptus oil raw material (eucalyptus oil containing 70% by mass percent 1,8-cineole) in a temperature-controlled bath, cool down to -19°C and stabilize for 5 minutes, add seed crystals (seed crystals are Prepared by freezing 1,8-cineole with a purity of 99.7% at -10°C), after continuing to stabilize for 10 minutes, cool down to -28°C at a cooling rate of 3°C / h, and after stabilizing for 30 minutes, filter and separate Obtain crude crystal and mother liquor, wherein the addition of crystal seed is 0.4% of the eucalyptus oil raw material quality;
[0037](2) Heating the crude crystals at a heating rate of 6°C / h, collecting sweat at every 3°C rise in temperature, raising the temperature to -8°C, and separating the sweat to obtain a primary crystallization product with a purity of 89.24% and a yield of ...
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