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Continuous crystallization method of tetraacetylethylenediamine

A tetraacetylethylenediamine and crystallization technology, applied in the crystallization field of tetraacetylethylenediamine, can solve the problems of uneven product particles, different sizes, low production efficiency, etc., and achieve production efficiency and product quality and particle size control. improved effect

Active Publication Date: 2012-07-18
ZHEJIANG JINKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using the existing crystallization kettle, the crystallization is slow, the time is long, the production efficiency is low, and the product particles are uneven, the size is different, and the color is not good, which seriously affects the quality of the product

Method used

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  • Continuous crystallization method of tetraacetylethylenediamine
  • Continuous crystallization method of tetraacetylethylenediamine
  • Continuous crystallization method of tetraacetylethylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] After the tetraacetylethylenediamine synthesis reaction is over, control the material temperature to 120℃; the continuous crystallizer volume is 5000L, keep the material weight in the continuous crystallizer 4000kg; control the feed and discharge rate of 200kg / h, control the circulation pump flow rate of 1102kg / h, change The temperature difference between the inlet and outlet of the heater is 2℃, and the crystallization temperature is 10℃; the crystalline product is obtained by centrifugation, water washing and drying; the product adopts HLPC to detect purity and Lab mode to detect color.

Embodiment 2

[0029] Adjust the material flow rate of 400kg / h, control the flow rate of the circulating pump 22040kg / h, the temperature difference between the inlet and outlet of the heat exchanger is 2℃, and the other conditions are the same as in Example 1.

Embodiment 3

[0031] The rate of incoming and outgoing materials is 400kg / h, the flow rate of the circulating pump is 8040kg / h, the temperature difference between the inlet and outlet of the heat exchanger is 5°C, and the crystallization temperature is 20°C. The other conditions are the same as in Example 1.

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Abstract

The invention discloses a continuous crystallization method of tetraacetylethylenediamine. The method is characterized by comprising the following steps that: (a) after the synthesis reaction of tetraacetylethylenediamine is finished, reaction material enters a crystallization pre-cooling kettle, and the temperature of the material is kept at 100-140 DEGE C; (b) the material in the crystallization pre-cooling kettle is conveyed by a crystallization feed pump, mixed with the outer circulation material of a continuous crystallizer and then conveyed by an outer circulation pump 2 of a crystallizer, and enters a continuous crystallizer 1 through a heat exchanger 3; (c) the material in the crystallizer passes through an outer circulation material outlet 2.8 and the outer circulation pump 2 and the heat exchanger 3 to enter the crystallizer from the an outer circulation material inlet 2.9 to finish the outer circulation process; and (d) the material discharged from the crystallization system is conveyed into a centrifugal separation device by a crystallization discharge pump 4 from a crystal mush outlet 2.11, and the obtained solid is washed and dried to obtain the crystal of tetraacetylethylenediamine. Through the method disclosed by the invention, the high-purity pure white tetraacetylethylenediamine product can be directly obtained, continuous crystallization is realized, and the production efficiency and product quality are obviously improved.

Description

Technical field [0001] The invention relates to a crystallization method of tetraacetylethylenediamine, more specifically a process for continuous crystallization of tetraacetylethylenediamine, which can directly obtain a tetraacetylethylenediamine product with high purity and good color. Background technique [0002] Tetraacetylethylenediamine is prepared from diacetylethylenediamine and acetic anhydride in the presence of a catalyst. In addition to catalysts, diacetylethylenediamine, triacetylethylenediamine and tetraacetylethylenediamine, the reaction system also contains A small amount of colored impurities make the system appear brown or brown. In the US patent US4240980, activated carbon or activated clay was used to decolorize and then crystallized to obtain qualified products; European patent EP0484634 uses a recrystallization method to decolorize tetraacetyl ethylene diamine. The crude product needs to be refined, and the crude product tetraacetylethylenediamine is refin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D9/02
Inventor 宋盘龙张招福唐新张敏敏芦鸿武
Owner ZHEJIANG JINKE CHEM
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