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Separation and extraction method for caprolactam, cyclohexane carboxylic acid, cyclohexane carboxylic sulfonic acid and organic oil in waste liquid generated in caprolactam production by toluene method

A cyclohexacarboxylic acid sulfonic acid and extraction method technology, which is applied in the field of comprehensive utilization of caprolactam waste liquid, can solve the problems that the treatment method cannot be used for continuous treatment of waste water, poor fluidity, no recovery, etc., and achieve high combustion value, Significant economic benefits and pollution reduction effects

Inactive Publication Date: 2012-03-21
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] The methods in the above two documents reduce the pollution of the waste liquid to the environment and realize the comprehensive utilization of the waste liquid, but do not recover the components with higher value such as caprolactam and cyclohexyl carboxylic acid in the waste liquid, and there are still high energy consumption. The material has problems such as high viscosity and poor fluidity after dehydration, and the treatment method cannot be used for continuous treatment of wastewater

Method used

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  • Separation and extraction method for caprolactam, cyclohexane carboxylic acid, cyclohexane carboxylic sulfonic acid and organic oil in waste liquid generated in caprolactam production by toluene method
  • Separation and extraction method for caprolactam, cyclohexane carboxylic acid, cyclohexane carboxylic sulfonic acid and organic oil in waste liquid generated in caprolactam production by toluene method
  • Separation and extraction method for caprolactam, cyclohexane carboxylic acid, cyclohexane carboxylic sulfonic acid and organic oil in waste liquid generated in caprolactam production by toluene method

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Embodiment 1

[0035] First, use sodium hydroxide to adjust the pH value of the waste liquid to 8-9, use chloroform as the extractant to extract caprolactam, extractant: waste liquid=1:1, and the extraction temperature is 30°C under normal pressure conditions Then adjust the pH value of the waste liquid with concentrated hydrochloric acid to be 1-2, select toluene as the extractant to extract cyclohexacarboxylic acid, during extraction, extractant: waste liquid=3: 4, what the extraction temperature selects is 30 ℃. carried out under normal pressure conditions. The organic solvent with high boiling point is nitrogen nitrogen dimethylformamide (DMF), DMF:waste liquid=3:4.

[0036] Step 1: Extraction of Caprolactam (CPL)

[0037]Weigh 400g of waste liquid in a 1000ml single-necked flask, add 7g of NaOH to it, stir to completely dissolve NaOH, and measure its pH value to 8.8 with a pH meter, then add 400g of chloroform to the waste liquid, and place it in a water bath at 30°C with a rotation sp...

Embodiment 2

[0044] Except that there is no extraction process of cyclohexyl carboxylic acid in embodiment 1, other is the same as embodiment 1

Embodiment 3

[0046] Except that there is no extraction process of caprolactam in embodiment 1, other is the same as embodiment 1

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Abstract

The invention provides a separation and extraction method for caprolactam, cyclohexane carboxylic acid, cyclohexane carboxylic sulfonic acid and organic oil in waste liquid generated in caprolactam production by the toluene method, which not only resolves the problem of environment pollution by waste liquid but also effectively recovers industrial chemicals such as caprolactam, cyclohexane carboxylic acid, cyclohexane carboxylic sulfonic acid and the like in the waste liquid. Furthermore, obtained organic oil which is high in combustion value can be directly used as fuel, and the method is applicable to continuous treatment of a great quantity of industrial waste water.

Description

technical field [0001] The invention relates to a comprehensive utilization method for producing caprolactam waste liquid, which comprises a method for separating and extracting caprolactam, cyclohexyl carboxylic acid, cyclohexyl carboxylic acid sulfonic acid and organic oil in the waste liquid. technical background [0002] Caprolactam is an important organic chemical raw material, mainly used in the production of nylon fiber and nylon resin, and has a wide range of applications. [0003] The waste liquid produced by the production of caprolactam by the toluene method mainly comes from: after the oxidation of toluene, the material is separated from the toluene by distillation and rectification, and the toluene is separated from the acetic acid water through the decanter; the ammoxidation reaction generates nitric oxide, carbon dioxide Nitrogen and water, the aqueous solution containing dilute nitric acid separated by heat exchange; when the caprolactam is refined, it is con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C07D223/10C07C61/08C07C51/48C07C309/27C07C303/44C02F1/26C02F1/66C02F1/04C02F103/36
CPCY02A20/124
Inventor 段正康杨运泉马帅贺玉平李立南
Owner XIANGTAN UNIV