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Method for isolating carbazole from anthracene oil

A technology for carbazole and anthracene oil is applied in the field of separation of carbazole to achieve the effects of simplified separation process, simplified separation process and reduced toxicity

Inactive Publication Date: 2014-02-26
HENAN UNIV OF URBAN CONSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the influence of the traditional thermal processing mode, this technology is rarely used in the coal chemical industry, and there is no research and application report on the separation of carbazole using this technology.

Method used

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  • Method for isolating carbazole from anthracene oil
  • Method for isolating carbazole from anthracene oil
  • Method for isolating carbazole from anthracene oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The method for separating carbazole from anthracene oil in this embodiment includes the following steps:

[0036] (1) Take 0.2655g of crude anthracene. The quality analysis results of the main components in crude anthracene are shown in Table 1 below and figure 2 ;

[0037] (2) Prepare solvent system

[0038] The volume ratio is n-heptane: benzene: acetone: acetonitrile = 4.5:1:1:4.5. Take each solvent, mix it with ultrasonic and degas for 20min, let it stand overnight to make the two-phase solvent reach a full equilibrium, and separate the solvent system Store the upper and lower phases in a closed container;

[0039] (3) Check each line interface of the complete set of TBE-300B high-speed countercurrent chromatograph to ensure that the connection is correct. Use the upper phase of the solvent system as the stationary phase and use a constant flow pump to input the spiral tube column of the countercurrent chromatograph until the column is full; The counter-current chromatogr...

Embodiment 2

[0044] The method for separating carbazole from anthracene oil in this embodiment includes the following steps:

[0045] (1) Take 0.5331g of decrystallized anthracene oil, and the quality analysis results of the main components are shown in Table 2 below and Figure 4 ;

[0046] (2) According to the volume ratio as cyclohexane:benzene:acetone:ethanol=3:2:2:3, take each solvent, mix it with ultrasonic and degas for 20min, let it stand overnight to make the two-phase solvent reach full equilibrium, and separate Store the upper and lower phases of the solvent system in a closed container;

[0047] (3) The countercurrent chromatography device is the same as in Example 1. The decrystallized anthracene oil is dissolved in the lower phase, the preparation volume is 30mL, the circulating water bath temperature is controlled to 45℃, the mobile phase flow rate is 3mL / min, and the stationary phase flow rate is 20mL / min. In forward mode, the speed of the main engine is 500 rpm, and other operat...

Embodiment 3

[0053] The method for separating carbazole from anthracene oil in this embodiment includes the following steps:

[0054] (1) Take 0.5508g of anthracene oil, and the quality analysis results of its main components are detailed in Table 3 and Image 6 ;

[0055] (2) Prepare solvent system

[0056] The volume ratio is n-hexane: benzene: acetone: methanol=7:2:2:7. Take each solvent, mix it with ultrasonic and degas for 20 minutes, and let it stand overnight to make the two-phase solvent reach a full equilibrium. Store the upper and lower phases in a closed container;

[0057] (3) The countercurrent chromatography device is the same as in Example 1. The anthracene oil is dissolved in the lower phase, the preparation volume is 30mL, the circulating water bath temperature is controlled to 40℃, the mobile phase flow rate is 3mL / min, and the stationary phase flow rate is 20mL / min. Mode, the host speed is 700rpm, other operations are the same as in Example 1;

[0058] (4) Observe the detection ...

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Abstract

The invention discloses a method for isolating carbazole from anthracene oil and belongs to the field of deep processing technology of coal tar. The method employs countercurrent chromatography technology, and has the following advantages that: (1) the method is directly applicable to separation of carbazole from anthracene oil, crude anthraene, decrystalized anthracene oil and the like, isolated carbazole contains a little amount of aromatic nitrogen-containing compounds, and high-purity carbazole with purity of 98% or more can be obtained after the isolated carbazole is recrystallized with xylene; (2) a to-be isolated sample can be fully contacted with a liquid-state stationary phase, and the method has the advantages of being no loss in sample, efficient, rapid, large in isolating amount, high in recovery rate and the like; (3) the boiling point of a solvent system is medium, so that the toxicity is substantially reduced, also airtight operation can be performed in the chromatogram system, there is no pollution, the sample is recoverable almost completely, and the solvents of stationary phase and mobile phase are recoverable and reusable; and (4) the isolation process of carbazole is simplified substantially, and the separation technology of anthracene oil, crude anthracene and the like is simplified.

Description

Technical field [0001] The invention specifically relates to a method for separating carbazole from anthracene oil, and belongs to the technical field of coal tar deep processing. Background technique [0002] Carbazole (C 12 H 9 N) is an important dye and pigment intermediate, and also an important raw material for synthetic resins. N-substituted carbazole synthesized with carbazole as the base material has special applications in light-guiding and conductive special polymer materials. Carbazole is also an important raw material for precious metal ore flotation agent, water reducer, stabilizer of lubricating oil and heat transfer oil, surfactant, fluorescent plasticizer, and biologically active material preparation. [0003] Carbazole is one of the important components in coal tar. It is enriched in the anthracene oil fraction along with anthracene and phenanthrene in the process of coal tar distillation. The anthracene oil is cooled and crystallized to obtain crude anthracene, wh...

Claims

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Application Information

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IPC IPC(8): C07D209/86C07D209/84
CPCC07D209/84C07D209/86
Inventor 丁明洁王宁苏箐刘泉龙赵辉赵静康
Owner HENAN UNIV OF URBAN CONSTR
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