Refined anthracene and carbazole purification method

A purification method and carbazole technology are applied in the field of continuous, rapid and efficient purification of refined anthracene and carbazole, which can solve the problems of large solvent consumption, low product yield and product quality, and increased extraction times, etc. The effect of few operation steps and high degree of automation

Inactive Publication Date: 2014-06-25
SHANGHAI YUGAO ENVIRONMENTAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: 1) This method is to increase the number of extractions to improve product quality, the production scale is small, the solvent consumption is large, and the product yield and product quality are low; 2) There are potential safety hazards in the process; 3) Other impurities are not used rationally, which is easy to pollute the environment
However, this method has the following disadvantages: 1) A part of anthracene and carbazole will be lost in impurities such as phenanthrene and fluorene; 2) The equipment is often bulky and requires a huge investment

Method used

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  • Refined anthracene and carbazole purification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The purification method of refined anthracene and carbazole provided in this embodiment, the steps are:

[0046]Step 1. Add 75kg of crude anthracene raw material into xylene, wherein the quality of xylene is 150kg, heat to 80°C to completely dissolve, cool down, let the solvent mother liquor stand at 20°C until complete crystallization, filter, and vacuum-dry the filter cake, Obtain 31kg of semi-refined anthracene and crude anthracene mother liquor, the crude anthracene mother liquor can replace xylene to dissolve subsequent crude anthracene raw materials, again make new semi-refined anthracene and crude anthracene mother liquor under the conditions of step 1, and repeat the above process for the crude anthracene mother liquor until the crude anthracene mother liquor The anthracene mother liquor is saturated, and the saturated crude anthracene mother liquor can be used as fuel oil.

[0047] Step 2, add 31kg of semi-refined anthracene in step 1 to DMF, wherein the qualit...

Embodiment 2

[0051] The purification method of refined anthracene and carbazole provided in this embodiment, the steps are:

[0052] Step 1. Add 750kg of crude anthracene raw material into xylene, wherein the quality of xylene is 1500kg, heat to 80°C to completely dissolve, cool, let the solvent mother liquor stand at 20°C until it is completely crystallized, filter, and dry the filter cake in vacuum. Obtain 307kg of semi-refined anthracene and crude anthracene mother liquor, the crude anthracene mother liquor can replace xylene to dissolve subsequent crude anthracene raw materials, again make new semi-refined anthracene and crude anthracene mother liquor under the conditions of step 1, the crude anthracene mother liquor repeats the above process until the crude anthracene mother liquor The anthracene mother liquor is saturated, and the saturated crude anthracene mother liquor can be used as fuel oil.

[0053] Step 2, add 307kg of semi-refined anthracene in step 1 to DMF, wherein the quali...

Embodiment 3

[0057] The purification method of refined anthracene and carbazole provided in this embodiment, the steps are:

[0058] Step 1. Add 750kg of crude anthracene raw material to toluene, wherein the mass of toluene is 1400kg, heat to 80°C to completely dissolve, cool, let the solvent mother liquor stand at 20°C until it is completely crystallized, filter, and dry the filter cake in vacuum to obtain 310kg Semi-refined anthracene and crude anthracene mother liquor, the crude anthracene mother liquor can replace toluene to dissolve subsequent crude anthracene raw materials, and then prepare new semi-refined anthracene and crude anthracene mother liquor under the conditions of step 1 again, and the crude anthracene mother liquor repeats the above process until the crude anthracene mother liquor is saturated , the saturated crude anthracene mother liquor can be used as fuel oil.

[0059] Step 2, add 310kg of semi-refined anthracene in step 1 to DMF, wherein the quality of DMF is 750kg,...

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Abstract

The invention relates to a refined anthracene and carbazole purification method. The purification method comprises the following steps: crystallizing and separating crude anthracene in a solvent I by adopting a solvent extraction and crystallization process, wherein crystal substances are semi-refined anthracene and the solution is a crude anthracene mother liquid; dissolving the semi-refined anthracene in a solvent II, ending heating and dropwise adding a solvent III for precipitation, separating the crystal substances to obtain the refined anthracene of which the concentration is higher than 95%; adding a solvent IV into the filtrate for crystallization to obtain the carbazole and solvent filtrate, separating the solvent filtrate to obtain the solvents II, III and IV which are recyclable, dissolving the carbazole into the solvent I for recrystallization, and separating final carbazole solids to obtain the carbazole of which the concentration is higher than 96%, wherein the crude anthracene mother solution and the carbazole filtrate can be used for replacing the solvent I for the crystallization of the semi-refined anthracene so as to realize recycling, and after saturation, the crude anthracene mother liquid and the carbazole filtrate can be used as fuel oil. The method is simple to operate, high in separation efficiency and free of generation of wastes during the whole reaction process.

Description

technical field [0001] The invention relates to a method for purifying refined anthracene and carbazole, in particular to a method for continuously, rapidly and efficiently purifying refined anthracene and carbazole. Background technique [0002] Anthracene is a condensed ring aromatic hydrocarbon with three rings, molecular formula C 14 h 10 . It is found in coal tar. Anthracene is a colorless flaky crystal with blue-violet fluorescence; melting point 216°C, boiling point 340°C, relative density 1.283; easily sublimated; insoluble in water, hardly soluble in ethanol and ether, easily soluble in hot benzene. The chemical activity of the 9 and 10 positions in the anthracene molecule is relatively high, and it can be oxidized with nitric acid to generate 9,10-anthraquinone, which is an important intermediate for the synthesis of anthraquinone dyes; the main use of anthracene is to obtain anthraquinone through oxidation. Anthraquinone is a widely used dye intermediate. Anth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/84C07D209/86C07C15/28C07C7/14C07C7/00
CPCC07C7/005C07C7/14C07D209/84C07D209/86C07C15/28
Inventor 江举辉陆阳王英杰
Owner SHANGHAI YUGAO ENVIRONMENTAL TECH CO LTD
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