Method for extracting fluorene, anthracene and carbazole from mixed anthracene oil

A technology of anthracene oil and carbazole, applied in organic chemistry, distillation purification/separation, crystallization purification/separation, etc., to achieve the effect of stable work

Active Publication Date: 2010-07-28
QUJING ZHONGYI SYNTHETIC CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A factory has been using furfural and heavy aromatics (heavy benzene) as solvents, but there are many problems. For this reason, a research institute of a coking plant in Beijing has researched and developed a single aprotic solvent, dimethylformamide (DMF), which can obtain a purity greater than 90% refined anthracene, and the yield is more than 20% higher than the original process, but the purity of the refined anthracene obtained by using a single DMF as a solvent is relatively high, but the extraction rate of anthracene is only about 50% compared with the crude anthracene

Method used

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  • Method for extracting fluorene, anthracene and carbazole from mixed anthracene oil
  • Method for extracting fluorene, anthracene and carbazole from mixed anthracene oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A. Rectification of mixed anthracene oil: The raw material mixed anthracene oil contains 6% acenaphthene, 4% oxyfluorene, 9% fluorene, 25% phenanthrene, 6% anthracene and 3% carbazole, and the flow rate of the raw material is 6253kg / h. After being heated to 150°C by the heating furnace of the oil washing tower, it enters the oil washing tower; the pressure at the top of the oil washing tower is 100kPa, the temperature is 260°C, the flow rate of the oil washing fraction is 1630kg / h, and the composition is 22% acenaphthene, oxygen Fluorene 14%, fluorene 32%; the washing oil fraction enters the fluorene tower, the pressure at the top of the fluorene tower is 20kPa, the temperature is 145°C, the flow rate of the naphthalene and methylnaphthalene fractions before the extraction of oxyfluorene is 455kg / h, and the fluorene The temperature of the upper side line of the tower is 185°C, the flow rate of the extracted fluorene fraction is 507kg / h, the temperature of the lower side ...

Embodiment 2

[0031] A. Rectification of mixed anthracene oil: the same raw material mixed anthracene oil as in Example 1, with a flow rate of 6350 kg / h. After preheating to 140°C, it enters the oil washing tower, the pressure at the top of the oil washing tower is 105kPa, the temperature is 265°C, and the flow rate of the extracted oil washing fraction is 1550kg / h; the washing oil fraction enters the fluorene tower, the fluorene tower The top pressure is controlled at 22kPa, the temperature is 148°C, the flow rate is 428kg / h, the temperature of the upper side line of the fluorene tower is 189°C, and the flow rate of the extracted fluorene distillate is 404kg / h; the temperature of the lower side line of the fluorene tower is 203°C, and the fluorene fraction is extracted The flow rate is 412kg / h; the operating temperature at the bottom of the fluorene tower is 212°C, and the flow rate of the extracted carbon black oil fraction is 306kg / h; the pressure at the bottom of the oil washing tower is...

Embodiment 3

[0036] A. Rectification of mixed anthracene oil: the same raw material mixed anthracene oil as in Example 1, with a flow rate of 5050 kg / h. After preheating to 130°C, it enters the oil washing tower, the pressure at the top of the tower is 100kPa, the temperature at the top of the tower is 260°C, and the flow rate of the washed oil fraction is 1200kg / h; the washed oil fraction enters the fluorene tower, and the top of the fluorene tower The pressure is controlled at 18kPa, the operating temperature is 150°C, the flow rate is 235kg / h, the temperature of the upper side line of the fluorene tower is 190°C, and the flow rate of the dioxyfluorene fraction is 351kg / h; the temperature of the lower side line of the fluorene tower is 198°C, and the flow rate of the extracted fluorene fraction is The operating temperature at the bottom of the fluorene tower is 210°C, the flow rate is 185kg / h, and the carbon black oil fraction is produced; the pressure at the bottom of the oil washing tow...

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Abstract

The invention discloses a method for extracting fluorene, anthracene and carbazole from mixed anthracene oil, comprising the steps of mixed anthracene oil rectifying, fluorene static crystallization, semi-refined anthracene extraction from first anthracene oil, semi-refined anthracene rectifying for extracting refined anthracene and carbazole, i.e. carrying out three-tower separation on the mixedanthracene oil, extracting components such as wash oil fraction, first anthracene oil fraction, second anthracene oil fraction, and the like. A crystallization method is adopted to remove impurities in the anthracene fraction, and the product has high purity and high yield. The separation of the refined anthracene and the carbazole adopts efficient rectification under vacuum for extracting anthracene and the carbazole. The invention is a novel process flow organically combined by a plurality of process equipment, has the advantages of convenience, high efficiency and stable work, achieves thepurposes of extracting a plurality of precious industrial chemical raw materials such as fluorene, carbazole, refined anthracene, and the like from the mixed anthracene oil through a set of process, and greatly improves the utilization value of first anthracene oil fraction and second anthracene oil fraction in coal tar, wherein the integrated extraction rate of fluorene, anthracene and carbazolerespectively reach 66%, 62% and 55% relative to the mixed anthracene oil as raw materials. Moreover, the invention also has the advantages of high production automation degree, environmental friendliness, energy saving, emission reduction, and obvious social and economical benefit.

Description

technical field [0001] The invention belongs to the technical field of coal chemical industry, and in particular relates to a method for extracting fluorene, anthracene and carbazole by using mixed anthracene oil. Background technique [0002] The components produced during the distillation and separation of high-temperature coal tar include light oil, phenol oil, naphthalene oil, wash oil, mono-anthracene oil, di-anthracene oil, asphalt and other components, of which mono-anthracene oil and di-anthracene oil are extracted from fluorene, anthracene, The main raw material of carbazole, a typical composition of mixed anthracene oil is 8.54% fluorene, 24.52% phenanthrene, 7.39% anthracene, and 4.14% carbazole. The traditional process is to separate mono-anthracene oil and di-anthracene oil, crystallize with mono-anthracene oil to obtain crude anthracene, or directly use mono-anthracene oil to extract anthracene and carbazole. Half of the carbazole resources are in dianthracene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/567C07C15/28C07C7/04C07C7/14C07D209/86C07D209/84
Inventor 李桂成罗国林
Owner QUJING ZHONGYI SYNTHETIC CHEMICAL CO LTD
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