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A kind of separation and purification process of caprolactam

A technology of caprolactam and process, which is applied in the field of chemical separation, can solve the problems of increasing equipment and increasing process complexity, and achieve the effects of reducing load, suppressing the content of polar impurities, and optimizing the extraction operation process

Active Publication Date: 2020-08-28
SHANDONG TSINGCHUANG CHEMICALSCO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These new processes have added new processes, which require certain modifications to existing production equipment, adding equipment, and increasing the complexity of the process.

Method used

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  • A kind of separation and purification process of caprolactam
  • A kind of separation and purification process of caprolactam
  • A kind of separation and purification process of caprolactam

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Example 1: The extraction tower uses a turntable tower, and the back extraction tower uses a pulse sieve tray tower. The extractant is a mixed solution prepared with a mass ratio of toluene and n-octane of 3:1. For the extraction tower, the feed flow rate of amide oil is 10t / h, the feed flow rate of extractant is 40t / h, and the rotating speed of the turntable is 18 revolutions per minute. For the stripping tower, the feed flow rate of water is 6t / h, the pulse amplitude is 2cm, and the pulse frequency is 60 Hz. The dehydration tower uses a float valve tower and operates under normal pressure. The temperature of the bottom of the tower is 120°C and the temperature of the top of the tower is 95°C. The crude caprolactam rectification tower uses a packed tower, operating at 2.2 kPa (absolute pressure), and the bottom temperature of the tower is 145°C. The concentration of caprolactam in the loaded extractant discharged from the extraction tower is 14.8%wt. The caprolactam c...

Embodiment 2

[0032] Example 2: The extraction tower uses a pulse sieve plate tower, and the reverse extraction tower uses a pulse sieve plate tower. The extractant is a mixed solution prepared with a mass ratio of toluene and n-octane 2:1. For the extraction tower, the feed flow rate of amide oil is 10t / h, the feed flow rate of extractant is 60t / h, and the rotating speed of the turntable is 20 revolutions per minute. For the stripping tower, the water feed flow rate is 5.2t / h, the pulse amplitude is 2cm, and the pulse frequency is 60 Hz. The dehydration tower uses a float valve tower and operates under normal pressure. The temperature of the bottom of the tower is 120°C and the temperature of the top of the tower is 95°C. The crude caprolactam rectification tower uses a packed tower, operating at 2.0kPa (absolute pressure), and the temperature of the tower bottom is 140°C. The concentration of caprolactam in the loaded extractant discharged from the extraction tower is 9.8%wt. The caprola...

Embodiment 3

[0033] Example 3: The extraction tower uses a turntable tower, and the reverse extraction tower uses a turntable tower, and the extractant is a mixed solution prepared with a mass ratio of toluene and n-octane 1:1. For the extraction tower, the feed flow of amide oil is 10t / h, the feed flow of extractant is 80t / h, and the rotating speed of the turntable is 22 revolutions per minute. For the stripping tower, the water feed flow rate is 5t / h, the pulse amplitude is 2cm, and the pulse frequency is 60 Hz. The dehydration tower uses a float valve tower and operates under normal pressure. The temperature of the bottom of the tower is 120°C and the temperature of the top of the tower is 95°C. The crude caprolactam rectification tower uses a packed tower, operating at 1.8kPa (absolute pressure), and the bottom temperature of the tower is 135°C. The concentration of caprolactam in the loaded extractant discharged from the extraction tower is 7.5% wt. The caprolactam concentration in t...

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Abstract

The invention discloses a separating and refining process for caprolactam. According to the process, amide oil, containing 60-70wt% of caprolactam, obtained in caprolactam production is taken as a treatment object; the process is characterized in that a mixed solvent of arene and alkane is utilized as an extraction agent and the high-purity caprolactam is obtained only through dehydration and rectification after reverse extraction through improving the selectivity of the extraction and reverse extraction procedures and reducing reverse extraction water. Compared with the prior art, the separation procedures, such as steam stripping, ion exchange and triple-effect evaporation are concealed, the corresponding construction and operation cost is reduced, the energy consumption of the separation process, the caprolactam loss and the wastewater discharge are significantly reduced, and the process meets the development direction of green chemical industry.

Description

Technical field [0001] The invention belongs to the technical field of chemical separation, and particularly relates to a process for separating and refining caprolactam from amide oil containing caprolactam with the characteristics of simplicity, low consumption and low emission. Background technique [0002] Caprolactam is an important organic chemical raw material, mainly used as a chemical fiber monomer to make nylon 6. There are many production methods for caprolactam. The cyclohexanone-hydroxyamine method and cyclohexanone ammoximation method using benzene as the raw material are currently the mainstream. In both methods, cyclohexanone oxime is first prepared, and then the cyclohexanone oxime is subjected to Beckman rearrangement reaction under the action of oleum to obtain caprolactam. In order to remove fuming sulfuric acid in the reaction system, it is necessary to add water and gaseous ammonia to convert it into ammonium sulfate. Ammonium sulfate, caprolactam and water...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/10C07D201/16
CPCC07D201/16C07D223/10
Inventor 陈桂光
Owner SHANDONG TSINGCHUANG CHEMICALSCO LTD
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