Method for separating and purifying coenzyme Q<10> from coenzyme Q<10> mother liquor, and coenzyme Q<10> crud product
A separation and purification, coenzyme technology, applied in the field of chemical engineering, can solve the problems of high environmental protection cost, limited production, loss of production mother liquor, etc.
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Embodiment 1
[0053] The present embodiment provides a kind of from coenzyme Q 10 Separation and purification of coenzyme Q from mother liquor 10 method, which includes the following steps:
[0054] (1) Coenzyme Q 10 10L of the mother liquor was concentrated to 1L under reduced pressure at 60°C and 0.05MPa, and the concentrated solution was measured, coenzyme Q 10 Content 287.98mg / ml, purity 58.41%.
[0055] (2) Add 3 L of n-heptane to 1 L of concentrated solution, heat up and stir at 65° C. to dissolve, and obtain 4 L of solution. coenzyme Q 10 Titer 71.999mg / ml.
[0056] (3) Add water according to 0.2 times the volume of the solution, stir for 30 minutes, and let stand for 2 hours to separate layers to obtain a 3.9L n-heptane layer with a titer of 73.84mg / ml and a 1L water layer with a titer of 0.18mg / ml. ml, the washing yield was 98.64%.
[0057](4) The n-heptane layer is put on the packed silica gel column (manufacturer: Qingdao Meigao Group, key quality parameters of silica gel:...
Embodiment 2
[0061] (1) Coenzyme Q 10 13L of mother liquor was concentrated to 950ml at 65°C and 0.06MPa, and the concentrated liquid coenzyme Q 10 Content 249.59mg / ml, purity 56.00%.
[0062] (2) To 1 L of concentrated solution, 2 L of n-heptane was added, heated and stirred at 65° C. to dissolve, and 3 L of dissolved solution was obtained. coenzyme Q 10 Titer 74.877mg / ml.
[0063] (3) Add water according to 0.3 times the volume of the solution, stir for 30 minutes, and let stand for 2 hours to separate layers to obtain a 3L n-heptane layer with a titer of 73.19mg / ml in the n-heptane layer and 595ml of the water layer with a titer of 0.37mg / ml , the washing yield was 97.89%.
[0064] (4) The n-heptane layer is placed in the packed silica gel column according to 70mg / g, and the flow rate of the upper column is controlled at 0.5BV / h. After the upper column is finished, the silica gel column is prewashed with 5 times the volume of n-heptane, so that Remove the impurities as much as poss...
Embodiment 3
[0068] (1) Coenzyme Q 10 14L of mother liquor was concentrated to 1.2L at 69°C and 0.08MPa, and the concentration of coenzyme Q was measured 10 Content 212.79mg / ml, purity 65.41%.
[0069] (2) Add n-heptane to 1.2 L of concentrated solution, heat up and stir at 65°C to dissolve, and obtain 3 L of solution. coenzyme Q 10 Titer 70.93mg / ml.
[0070] (3) Add water according to 0.2 times the volume of the solution, stir for 30 minutes, and let stand for 2 hours to separate layers to obtain a 2.9L n-heptane layer with a titer of 70.73mg / ml and a water layer of 610mlL with a titer of 0.41mg / ml. ml, the washing yield was 96.39%.
[0071] (4) The n-heptane layer is placed on the packed silica gel column according to 70mg / g, and the flow rate of the upper column is controlled at 0.5BV / h. After the upper column is completed, the silica gel column is prewashed with 4 times the volume of n-heptane, so that Remove the impurities as much as possible, replace the n-heptane containing 7% ...
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