Method for continuously producing triacetonamine with high stability by using melt crystallization technology
A high-stability, triacetone-amine technology, applied in the direction of organic chemistry, can solve the problems of increased post-peak impurities, poor product stability, and increased solid waste, and achieve reduced residual impurities, stable quality, and simplified process flow Effect
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Embodiment 1
[0039]Such as figure 1 As shown, under the protection of nitrogen gas, 5 liters of glass melting crystallizer 2 is preheated to 60 ° C, and the content of injecting 3.5 kg in the melting crystallizer is 73.8% molten triacetone amine crude product (produced by Suqian Zhenxing Chemical Co., Ltd. , batch number 20140703), lower the temperature at a rate of 0.5°C per minute, drop to 20°C and keep for 1 hour, press out the unattached liquid with nitrogen to obtain 1.68kg of dark brown crystalline mother liquor B with a content of 55.1%, and press it into the crystallizer 1. Reheat the attached solid to 55° C. to melt, press out with nitrogen, measure, detect by GC, and enter to obtain 1.81 kg of light yellow triacetonamine semi-finished product with a content of 92.5%.
[0040] Then heat the above 1.81kg semi-finished product to 65°C, inject it into the 3-liter glass melting crystallizer 3 that has been preheated to 65°C under the protection of nitrogen, cool down at a rate of 0.4...
Embodiment 2
[0042] Such as figure 1 As shown, under the protection of nitrogen gas, 50 liters of stainless steel melting crystallizer 2 is preheated to 60 ° C, and 35 kg of molten triacetone amine crude product with a content of 74.1% is injected into the melting crystallizer (produced by Suqian Zhenxing Chemical Co., Ltd., batch number 20140705) , lowered the temperature at a rate of 0.5° C. per minute, dropped to 20° C. and kept for 2 hours, and the unattached liquid was depressurized with nitrogen to obtain 16.95 kg of dark brown solution B with a content of 55.7%. Then heated to 55° C. to melt the attached solid and press out with nitrogen to obtain 18.01 kg of light yellow triacetonamine semi-finished product with a content of 91.6%.
[0043] Then add the above 18.01kg semi-finished product into the 30-liter stainless steel melting crystallizer 3 preheated to 65°C, lower the temperature at a rate of 0.4°C per minute, drop it to 25°C and keep it for 2 hours, and press out the unattach...
Embodiment 3
[0045] Such as figure 1 As shown, under the protection of nitrogen gas, 3 liters of glass melting crystallizer 1 is preheated to 60°C, and 2.1kg of crystallization mother liquor B with a content of 55.1% is injected into the melting crystallizer 1, and the temperature is lowered at a rate of 0.3°C per minute. Keep at 15° C. for 2 hours, press out the unattached liquid with nitrogen to obtain 1.04 kg of dark brown crystalline mother liquor C with a content of 37.3% (the crystallized mother liquor C with this content is pressed into the synthesis section for processing). Then the temperature was raised to 55° C. to melt the attached solid and blow out with nitrogen pressure to obtain 1.05 kg of light brown crude triacetonamine with a content of 73.2% (the crude product with this content directly enters the crystallizer 2) for circulation.
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