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Method and device for extracting hexahydrobenzoic acid from rearrangement reaction liquid

A hexahydrobenzoic acid and rearrangement reaction technology, applied in the separation/purification of carboxylic acid compounds, etc., can solve the problems of sulfonation loss, gravity settling tank can not be used for separation time, large equipment investment and other problems

Active Publication Date: 2013-11-13
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] If a gravity settling tank is used to separate the amidation reaction liquid, there will be problems such as low separation efficiency, large equipment investment and long time required
Gravity settling tanks cannot be applied to occasions that require a short separation time. In the process of extracting CCA in the rearrangement reaction liquid with n-hexane, the longer the separation time, the greater the separation time between CCA and SO 3 The more severe the sulfonation, the greater the loss of CCA
Therefore, gravity settling tank cannot be used to extract and separate the CCA in the rearrangement reaction liquid
As far as the tower extraction equipment is concerned, its separation time is also longer, which will cause a certain degree of sulfonation loss, and its equipment cost and operating cost are also relatively expensive.
In addition, when the tower extraction equipment stops, the two-phase liquid balance will be destroyed, which will reduce the production efficiency
[0005] So far, the method for solving the above-mentioned technical problems has not been proposed in the prior art

Method used

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  • Method and device for extracting hexahydrobenzoic acid from rearrangement reaction liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] according to figure 1 The process flow shown carries out the separation of the amidation reaction liquid.

[0050] 1. Material properties

[0051] (1) Rearrangement reaction solution: the material is a mixture of organic phase and inorganic phase, and the content of CCA fluctuates between 20-25%. The rated flow rate is 20 tons / hour, the temperature is 60-80°C, the average temperature is about 70°C, and the density is 1270kg / m 3 , the viscosity is 263mpa·s.

[0052] (2) n-Hexane: flow rate 2.0 tons / hour, temperature 50-60°C, average temperature about 57°C, density 761kg / m 3 , the viscosity is 0.26mpa·s.

[0053] 2. The motor speed of the centrifugal extractor is 900 rpm.

[0054] 3. Content determination method:

[0055] Using gas chromatography.

[0056] 4. Application effect

[0057] (1) 2.0 tons / hour of n-hexane at normal temperature is added, the content of the light phase in the heavy phase after separation is less than 1%, and the content of the heavy phase...

Embodiment 2

[0060] according to figure 1 The process flow shown carries out the separation of the amidation reaction liquid.

[0061] 1. Material properties

[0062] (1) Rearrangement reaction solution: the material is a mixture of organic phase and inorganic phase, and the content of CCA fluctuates between 20-25%. The rated flow rate is 20 tons / hour, the temperature is 60-80°C, the average temperature is about 70°C, and the density is 1270kg / m 3 , the viscosity is 263mpa·s.

[0063] (2) n-Hexane: The flow rate is 4.0 tons / hour, the temperature is 50-60°C, the average temperature is about 57°C, and the density is 761kg / m 3 , the viscosity is 0.26mpa·s.

[0064] 2. The motor speed of the centrifugal extractor is 900 rpm.

[0065] 3. Content determination method

[0066] Using gas chromatography.

[0067] 4. Application effect

[0068] (1) 4.0 tons / hour of normal-temperature n-hexane is added, the content of the light phase in the heavy phase after separation is less than 0.8%, and ...

Embodiment 3

[0071] according to figure 1 The process flow shown carries out the separation of the amidation reaction liquid.

[0072] 1. Material properties

[0073] (1) Rearrangement reaction solution: the material is a mixture of organic phase and inorganic phase, and the content of CCA fluctuates between 20-25%. The rated flow rate is 20 tons / hour, the temperature is 60-80°C, the average temperature is about 70°C, and the density is 1270kg / m 3 , the viscosity is 263mpa·s.

[0074] (2) n-Hexane: The flow rate is 8.0 tons / hour, the temperature is 50-60°C, the average temperature is about 57°C, and the density is 761kg / m 3 , the viscosity is 0.26mpa·s.

[0075] 2. The motor speed of the centrifugal extractor is 900 rpm.

[0076] 3. Content determination method

[0077] Using gas chromatography.

[0078] 4. Application effect

[0079] (1) 8.0 tons / hour of n-hexane at normal temperature is added, the content of the light phase in the heavy phase after separation is less than 0.5%, a...

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Abstract

The invention relates to a method and device for extracting hexahydrobenzoic acid from a rearrangement reaction liquid, and provides the method for extracting hexahydrobenzoic acid from the rearrangement reaction liquid. The method comprises the steps of: (a) conveying the rearrangement reaction liquid from a rearrangement reactor to a heavy phase inlet of a centrifugal extractor, conveying n-hexane to a light phase inlet of the centrifugal extractor, carrying out sufficient mixing and mass transfer on the rearrangement reaction liquid and n-hexane between a high-speed rotating inner drum and a stationary outer drum of the centrifugal extractor, thus extracting hexahydrobenzoic acid from the rearrangement reaction liquid to n-hexane; (b) carrying out liquid-liquid separation on the mixed liquid of the rearrangement reaction liquid and n-hexane with the centrifugal extractor to form a light phase rich in hexahydrobenzoic acid and a heavy phase with hexahydrobenzoic acid removed; and (c) conveying the obtained heavy phase to a hydrolysis reactor for hydrolyzing, then conveying to a sedimentation tank, and directly conveying the obtained light phase to the sedimentation tank. The invention also provides the device for extracting hexahydrobenzoic acid from the rearrangement reaction liquid.

Description

technical field [0001] The invention relates to a method and a device for extracting and separating rearrangement reaction liquid CCA (hexahydrobenzoic acid) in caprolactam production. More specifically, it relates to a method and device for extracting and separating the rearrangement reaction liquid CCA in the production of caprolactam by using a centrifugal extractor. Background technique [0002] The combined process of hexahydrobenzoic acid-cyclohexanone oxime co-production of caprolactam is a caprolactam production process developed by my country, which includes biomimetic catalytic oxidation of cyclohexane, ammoximation of cyclohexanone, gas phase rearrangement of cyclohexanone oxime, hydrolysis, Neutralization, refining and other process links. Hexahydrobenzoic acid (CCA) is an important raw material for the production of caprolactam by combined process. During the gas phase rearrangement of cyclohexanone oxime to the hydrolysis process, since the rearrangement react...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C61/08C07C51/48
Inventor 白志山唐康郝萌萌
Owner EAST CHINA UNIV OF SCI & TECH
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