Method for cooling, crystallizing and separating 4-cyanopyridine by solvent
A cyanopyridine, cooling crystallization technology, applied in the direction of organic chemistry and the like, can solve the problems of low recycling rate, waste of environment, pollution, etc., and achieves the effect of solving waste recycling, low production cost and good economic benefits
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Embodiment 1
[0019] The mixed cyanopyridine raw material containing 3-cyanopyridine and 4-cyanopyridine is decolorized in a decolorization device at 80°C, and then the filtered filtrate is added to methanol to prepare a cyanide with a supersaturation of 0.05 at 45°C The solution was continuously stirred at a stirring rate of 150 rpm, the crystallization temperature dropped from 50°C to 5°C, and the cooling rate was 0.05°C / min. The crystals precipitated from the final filter were 99.4% high-purity 4-cyanopyridine products.
Embodiment 2
[0021] According to the conditions and steps described in Example 1, the supersaturation of the solution at 45°C was changed to 0.1, the stirring rate was 150rpm, the crystallization temperature was lowered from 50°C to 5°C, the cooling rate was 0.05°C / min, and finally the filter precipitated The crystals are 99.5% high-purity 4-cyanopyridine products.
Embodiment 3
[0023] According to the conditions and steps described in Example 1, the supersaturation of the solution at 45°C was changed to 0.2, the stirring rate was 150rpm, the crystallization temperature was reduced from 50°C to 5°C, the cooling rate was 0.05°C / min, and finally the filter precipitated The crystals are 99.4% high-purity 4-cyanopyridine products.
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