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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, low production efficiency, different sizes, etc., and achieve production efficiency and product quality and particle size control. improved effect

Active Publication Date: 2014-08-27
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 synthetic reaction of tetraacetylethylenediamine is completed, the temperature of the material is controlled at 120°C; the volume of the continuous crystallizer is 5000L, and the weight of the material in the continuous crystallization tank is kept at 4000kg; The temperature difference between the inlet and outlet of the heater is 2°C, and the crystallization temperature is 10°C; the crystalline product is obtained by centrifugation, washing, and drying; the purity of the product is tested by HLPC, and the color is tested by Lab mode.

Embodiment 2

[0029] Adjust the rate of incoming and outgoing materials to 400kg / h, control the flow rate of the circulation pump to 22040kg / h, and the temperature difference between the inlet and outlet of the heat exchanger to 2°C, and the rest of the conditions are the same as in Example 1.

Embodiment 3

[0031] The rate of incoming and outgoing materials was controlled to 400kg / h, the flow rate of the circulating pump was 8040kg / h, the temperature difference between the inlet and outlet of the heat exchanger was 5°C, and the crystallization temperature was 20°C. The rest of the conditions were 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 continuous crystallization process of tetraacetylethylenediamine, which can directly obtain tetraacetylethylenediamine products with high purity and good color. Background technique [0002] Tetraacetylethylenediamine is prepared by diacetylethylenediamine and acetic anhydride in the presence of a catalyst. In addition to the catalyst, there are diacetylethylenediamine, triacetylethylenediamine and tetraacetylethylenediamine in the reaction system, there will also be A small amount of colored impurities make the system brown or brown. In U.S. Patent No. 4,240,980, the method of adding activated carbon or activated clay was used for decolorization, and then crystallized to obtain qualified products; The crude product needs to be refined, and the crude product tetraacetylethylenediamine is refined. These operations have increased production equipment inv...

Claims

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Application Information

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Patent Type & Authority Patents(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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