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Industrial purification method of hexamethylenediamine

A purification method and technology of hexamethylenediamine, applied in the direction of amino compound purification/separation, organic chemistry, etc., can solve the problem of high energy consumption for purifying hexamethylenediamine, and achieve the effect of less heat and low energy consumption

Pending Publication Date: 2022-06-28
SHANGHAI DONGGENG CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of the above-mentioned shortcomings of the prior art, the purpose of the present invention is to provide a method for industrial purification of hexamethylenediamine, which is used to solve the problem of high energy consumption in the purification of hexamethylenediamine by rectification process in the prior art

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  • Industrial purification method of hexamethylenediamine
  • Industrial purification method of hexamethylenediamine
  • Industrial purification method of hexamethylenediamine

Examples

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Embodiment 1

[0053] like figure 1 and figure 2 As shown, this embodiment provides an industrial purification method for hexamethylene diamine, which adopts a three-stage crystallization method in a falling film crystallizer, and specifically includes the following steps:

[0054] Step 1, stirring and evaporation: using stirring evaporator 1, the adiponitrile hydrogenation reaction product (liquid material containing hexamethylene diamine) was stirred and evaporated at 79 ° C for 20 min, and the ethanol in the adiponitrile hydrogenation reaction product was removed. remove.

[0055] Step 2: Pre-cooling and crystallization: use the micro-melt crystallizer 2 to carry out pre-cooling and crystallization, combined with image 3 As shown, the micro-melt crystallizer 2 includes a shell 16, and the inner space of the shell 16 is communicated with a cooling and heating medium inlet pipe 17 and a cooling and heating medium outlet pipe 18. The casing 16 is provided with a number of crystalline tu...

Embodiment 2

[0066] The only difference between this example and Example 1 is that this example follows the method of Example 1, and in Step 1, the time for stirring and evaporating is 25 minutes.

[0067] In step 2, the temperature of the cooling and heating medium is reduced at a rate of 15-25°C / h, and the temperature of the liquid material is slowly reduced to 63°C within 38-60 minutes.

[0068] In step three (a), the cooling and heating medium is cooled at a rate of 20-30°C / h, and the liquid material is cooled to 40.5°C within 45-68 minutes; h Raise the temperature of the cooling and heating medium to 42°C, heat for 15 minutes, and keep the cooling and heating medium at 42°C for 15 minutes.

[0069] In step 4, the temperature of the liquid material is slowly reduced to about 40.5°C within 45 minutes, then the temperature of the cooling and heating medium is raised to 42.5°C at 6°C / h, heated for 20 minutes, and the cooling and heating medium is kept at 42.5°C for 15 minutes in circulati...

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Abstract

The invention belongs to the technical field of material purification, and particularly discloses a hexamethylenediamine industrial purification method which comprises the following steps: 1) pre-cooling crystallization: cooling an adiponitrile hydrogenation reaction product from 70-100 DEG C to 55-63 DEG C for primary crystallization, separating crystals from a liquid material, and collecting the liquid material; 2) melt crystallization: adopting a falling film crystallizer to cool the liquid material in the step 1) to 35-40 DEG C for crystallization; 3) partial melting: raising the temperature to 42-43 DEG C, and collecting sweating liquid; 4) melting: raising the temperature to 55 DEG C or above, and collecting molten liquid as a feeding material for next-stage crystallization; and (5) repeating the steps (2)-(4) for 1-3 times to perform multistage crystallization, collecting molten liquid, and cooling and crystallizing to obtain the high-purity hexamethylenediamine. According to the method, hexamethylenediamine with the purity of 99.99% can be obtained through pre-cooling crystallization and multi-stage crystallization, the energy consumption of the method is lower than that of hexamethylenediamine purified through a rectification process, and the requirements of energy conservation and environmental protection are better met.

Description

technical field [0001] The invention relates to the technical field of material purification, in particular to an industrial purification method of hexamethylenediamine. Background technique [0002] Hexanediamine, alias 1,6-diaminohexane, 1,6-hexanediamine, is one of the important raw materials for chemical synthesis, mainly used for the production of nylon 66 and 610 resins, and can be used to make adhesives and rubber products additives, stabilizers, bleaching agents, coatings, etc. in the textile and paper industry. The main production methods of hexamethylene diamine include adiponitrile method, hexanediol method, caprolactam method, adipic acid method, butadiene method, etc. Among them, caprolactam method and butadiene method are only suitable for small-scale production, and because of the production The cost is high and is gradually eliminated, while the adiponitrile method is widely used because of its simple process, high product quality and low production cost. Th...

Claims

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Application Information

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IPC IPC(8): C07C209/84C07C211/12
CPCC07C209/84C07C211/12
Inventor 丁永良张飞陈孝建钟显威李明全贾凤刚
Owner SHANGHAI DONGGENG CHEM TECH CO LTD
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