A kind of fine purification method of isoquinoline
A purification method and isoquinoline technology, applied in the direction of organic chemistry and the like, can solve the problems of complicated operation, unsatisfactory purification effect, long consumption time, etc., and achieve the effects of short consumption time, easy industrial control, and simple operation.
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Embodiment 1
[0021] Isoquinoline purification steps:
[0022] (1) Set 2.0M 3 Concentration is 73.46% isoquinoline enrichment solution (wherein water content is 0.05%), isothermally crystallized at 5 ℃ for 24 hours, and the crystallization mother liquor is evacuated by vacuum filtration (vacuum degree is 0.05kg / cm 2 ).
[0023] (2) Sweat for 4 times, and discharge after heating and melting; the sweating conditions are: 10°C isothermal for 6 hours, 15°C for 6 hours, 20°C for 6 hours, 25°C for 24 hours, vacuum filtration after each isotherm Empty sweating mother liquor (vacuum degree is 0.05kg / cm 2 , discharge rate 1% / hour).
[0024] (3) Detect crystallization mother liquor and sweating mother liquor. The crystallization mother liquor contains 61.54% isoquinoline, and is stored as a standard material of 50% to 70% isoquinoline. At 10°C, 15°C, and 20°C, the sweating mother liquor contains 71.62%, 78.72%, and 87.52% isoquinoline, respectively, and is stored as the standard material of 70%-...
Embodiment 2
[0029] Isoquinoline purification steps:
[0030] (1) Set 2.0M 3 Concentration is 71.56% isoquinoline enrichment solution (wherein water content is 0.05%), isothermally crystallized at 0 ℃ for 24 hours, and the crystallization mother liquor is evacuated by vacuum filtration (vacuum degree is 0.8kg / cm 2 ).
[0031] (2) Sweat for 5 times, and discharge after heating and melting; the sweating conditions are: isothermal at 5°C for 6 hours, 10°C for 6 hours, 15°C for 6 hours, 20°C for 6 hours, and 25°C for 24 hours. After the end, vacuum filter and evacuate the sweating mother liquor (vacuum degree is 0.8kg / cm 2 , discharge rate 0.5% / hour).
[0032] (3) Detect crystallization mother liquor and sweating mother liquor. The crystallization mother liquor contains 53% isoquinoline, and is stored as a standard material of 50%-70% isoquinoline. At 5°C, 10°C, 15°C, and 20°C, the sweating mother liquor contained 70.36%, 72.29%, 78.48%, and 84.91% of isoquinoline, respectively, and was s...
Embodiment 3
[0037] Isoquinoline purification steps:
[0038] (1) Set 2.0M 3 Concentration is 70.92% isoquinoline enrichment solution (wherein water content is 0.05%), isothermally crystallized at 0 ℃ for 48 hours, and the crystallization mother liquor is evacuated by vacuum filtration (vacuum degree is 0.8kg / cm 2 ).
[0039] (2) Sweat for 5 times, and discharge after heating and melting; the sweating conditions are: isothermal at 5°C for 6 hours, 10°C for 6 hours, 15°C for 6 hours, 20°C for 6 hours, and 25°C for 12 hours. After the end, vacuum filter and evacuate the sweating mother liquor (vacuum degree is 0.8kg / cm 2 , discharge rate 0.75% / hour).
[0040] (3) Detect crystallization mother liquor and sweating mother liquor. The crystallization mother liquor contains 56% isoquinoline, and is stored as a standard material of 50% to 70% isoquinoline. The sweating mother liquors at 5°C, 10°C, 15°C, and 20°C contained 70.63%, 75.86%, 80.28%, and 85.41% isoquinoline, respectively, and were...
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