Neutralized crystallization system and method of preparing caprolactam through caprolactam rearrangement solution

A caprolactam, crystallization system technology, applied in the separation/purification of lactam, chemical instruments and methods, ammonia compounds, etc., can solve the problems of unreasonable energy utilization, consumption of cooling and heat, heating, etc., to shorten the process flow and Equipment investment, heat and cooling effect

Inactive Publication Date: 2013-04-03
SEDIN NINGBO ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the ammonia neutralization reaction is completed, to obtain caprolactam and ammonium sulfate products, it is necessary to evaporate the water added and reacted in the system. Since the neutralization process and the water evaporation process are carried out separately, the heat released during the neutralization reaction The loss needs to be taken away by coo

Method used

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  • Neutralized crystallization system and method of preparing caprolactam through caprolactam rearrangement solution

Examples

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Embodiment 1

[0025] A kind of caprolactam rearrangement liquid of the present invention prepares the neutralization crystallization system of caprolactam, such as figure 1 Shown, comprise feed mixer 1, neutralization crystallization reactor 2, caprolactam oil stratifier 3, ammonium sulfate centrifuge 4, ammonium sulfate washing drier 5, ammonium sulfate mother liquor collection tank 6 and caprolactam collection tank 7, carry out The material mixer 1 is connected with the upper inlet of the neutralization crystallization reactor 2, the upper layer light organic phase outlet of the neutralization crystallization reactor 2 is connected with the inlet of the caprolactam oil stratifier 3, and the lower layer heavy organic phase of the neutralization crystallization reactor 2 Outlet 14 is connected with the inlet of ammonium sulfate centrifuge 4, and one end outlet of caprolactam oil stratifier 3 is connected with caprolactam collection tank 7, and the other end outlet is connected with ammonium ...

Embodiment 2

[0029] A kind of caprolactam rearrangement liquid of the present invention prepares the method for caprolactam, such as figure 1 As shown, it specifically includes the following steps:

[0030] (1) Send the caprolactam rearrangement liquid, ammonia and water into the feed mixer 1 with a mass ratio of 1:3:2.5 and mix them evenly, then send them to the neutralization crystallization reactor 2 for neutralization reaction, and the heat generated by the reaction makes the water Evaporate, reduced reaction temperature simultaneously, after neutralization reaction 5 minutes, the liquid in the neutralization crystallization reactor 2 is divided into the first light organic phase of the upper floor and the first heavy organic phase of the lower floor, wherein the operating pressure of the neutralization crystallization reactor 2 -0.095MPaG, operating temperature is 50°C;

[0031] (2) Extract the first light organic phase from the upper part of the neutralization crystallization reacto...

Embodiment 3

[0037] The same as Example 2, the difference is that in step (1), the caprolactam rearrangement liquid, ammonia and water are sent to the feed mixer 1 at a mass ratio of 1:3.5:2.75 and mixed evenly, and then sent to the neutralization crystallization reactor 2 The neutralization reaction occurred, and after 10 minutes of the neutralization reaction, the operating pressure of the neutralization crystallization reactor 2 was -0.07MPaG, and the operating temperature was 70°C.

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Abstract

The invention discloses neutralized crystallization system and method of preparing caprolactam through caprolactam rearrangement solution. The neutralized crystallization system is characterized in that a feeding mixer is connected with an inlet in the upper part of a neutralized crystallization reactor, an upper-layer organic phase outlet of the neutralized crystallization reactor is connected with an inlet of a caprolactam oil layer separator, a lower-layer heavy organic phase outlet of the neutralized crystallization reactor is connected with an inlet of an ammonium sulfate centrifugal machine, an outlet at one end of the caprolactam oil layer separator is connected with a caprolactam collecting tank, an outlet at the other end of the caprolactam oil layer separator is connected with an ammonium sulfate mother liquor collection tank, an outlet at the lower end of the ammonium sulfate centrifugal machine is connected with an ammonium sulfate washing dryer, an outlet at the upper end of the ammonium sulfate centrifugal machine is connected with the ammonium sulfate mother liquor collection tank which is connected with the neutralized crystallization reactor through a mother liquor circulating pump. The neutralized crystallization system and method have the advantages that the heating and cooling capacities are integrated in reaction process, the energy consumption is low, the process is simple, and the purity of the product is high.

Description

technical field [0001] The invention relates to a preparation method of caprolactam, in particular to a neutralization crystallization system and method for preparing caprolactam from caprolactam rearrangement liquid. Background technique [0002] Caprolactam is one of the important raw materials for synthetic fibers and synthetic materials. It is mainly used in the manufacture of polyamide 6 fibers (nylon 6), resins and films. Chemically synthesized lysine has a wide range of uses in many fields such as textiles, plastics, and fine chemicals. The Beckmann rearrangement reaction of cyclohexanone oxime is the most important process in the production process of caprolactam, which plays a key role in product quality. [0003] At present, the industrial production of caprolactam rearrangement liquid (caprolactam sulfate) is obtained by rearranging cyclohexanone oxime under the action of oleum with concentrated sulfuric acid or oleum as a catalyst, and then the caprolactam rearr...

Claims

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Application Information

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IPC IPC(8): C07D233/10C07D201/16C01C1/242
Inventor 谷新春梁正王宇光颜焕敏马文华胡晓铮
Owner SEDIN NINGBO ENG
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