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A method for continuously producing high-stability triacetonamine using melt crystallization technology

A technology of triacetone amine and melt crystallization, applied in the direction of organic chemistry, etc., can solve the problems of poor product stability, increased post-peak impurities, decreased yield and other problems, and achieves the effects of stable quality, reduced residual impurities and less waste residue.

Active Publication Date: 2018-03-09
ZHENXING FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned methods all use complex equipment and high-temperature rectification will inevitably increase the rear peak impurities, resulting in decreased yield, increased solid waste and poor product stability.

Method used

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  • A method for continuously producing high-stability triacetonamine using melt crystallization technology
  • A method for continuously producing high-stability triacetonamine using melt crystallization technology
  • A method for continuously producing high-stability triacetonamine using melt crystallization technology

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to a method for continuously producing triacetonamine with high stability by using the melt crystallization technology. The method comprises the following steps: a), under the inert gas shielding environment, preheating a second melt crystallizer to the melting temperature, pouring molten triacetonamine crude products into the second melt crystallizer, cooling the second melt crystallizer to the crystallization temperature, and introducing inert gas to squeeze out unattached liquid; b), heating the second melt crystallizer to the melting temperature, melting attached solids, introducing inert gas to squeeze out molten attached solids, pouring molten attached solids into a third melt crystallizer which is preheated to the melting temperature, cooling the third melt crystallizer to the crystallization temperature, and introducing insert gas to squeeze out unattached liquid; c), heating the third melt crystallizer to the melting temperature, melting attached solids, and introducing insert gas to squeeze out molten attached solids, so as to obtain the triacetonamine with high stability.

Description

technical field [0001] The invention relates to a method for continuously producing high-stability triacetone amine by using melt crystallization technology. Background technique [0002] Triacetonamine is an important organic chemical intermediate with a chemical name of 2,2,6,6-tetramethylpiperidone. As the parent of hindered amine light stabilizer piperidine derivatives, it plays a fundamental role in the development of hindered amine light stabilizers, and can derive many very practical intermediates and hindered amine light stabilizers, such as 2, 2, 6 , 6-tetramethylpiperidinol, 1,2,2,6,6-pentamethylpiperidinol, light stabilizers 770, 944, 3346, etc.; especially high stability triacetone amine in the manufacture of 2,2 , 6,6-tetramethylpiperidine amine, piperidine hexamethylenediamine, 2,2,6,6-tetramethylpiperidine-4-oxyl radical and new light stabilizer NOR series products have obvious quality And cost advantages, with the wide application of light stabilizer NOR se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/74
CPCC07D211/74
Inventor 柯友斌张晓静李政伟
Owner ZHENXING FINE CHEM CO LTD
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