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Method for preparing refined anthracene by using coal tar as raw material

A technology of coal tar and refined anthracene, applied in the field of preparation of refined anthracene, can solve problems such as safety production and environmental protection difficulties, environmental pollution, flammability, etc., to avoid excessive loss of refined anthracene, improve economic value, and use less solvent Effect

Inactive Publication Date: 2012-10-24
韩钊武
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction methods of refined anthracene and carbazole mainly include solvent washing method (Guo Penghui, Hao Juanjuan. Progress in separation technology of anthracene, phenanthrene and carbazole in coal tar[J]. Hebei Chemical Industry, 2008, 31(11): 17-20.) and Combination of distillation and crystallization (Zhu Fubin, Chen Guangming. A new process for extracting refined anthracene and refined carbazole from anthracene oil [J]. Fuel and Chemical Industry, 2003, 34(6): 321-323.) two types of refining methods At present, the domestic production of refined anthracene and carbazole all adopts the solvent washing method. Although the solvents used are different, the principle is basically the same. Anthracene can only be recovered from the crude anthracene, and carbazole etc. are then discharged with the residual oil. Environmental pollution problems such as low efficiency and large solvent usage
The solvent method generally requires two kinds of solvents, and there are problems such as flammability, explosion and high volatility, and some solvents are also toxic, which brings certain difficulties to safe production and environmental protection
Even for the currently used refining method combining distillation and crystallization, although two products of anthracene and carbazole can be extracted from crude anthracene, there are still shortcomings such as low product yield and serious environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Step 1, the coal tar after the dehydration treatment is distilled at atmospheric pressure, and the fraction between 300 and 360 °C is cut;

[0020] Step 2, cooling all the fractions obtained in the step to room temperature, standing for crystallization at 10°C for 5 hours, to obtain an anthracene-carba mixture;

[0021] Step 3: Take 100 g of the anthracene-carbaphate mixture obtained in Step 2, add 200 g of xylene solution and 100 g of potassium hydroxide, and put them into a reactor connected with a water separator, stir and heat, heat and reflux to separate water until almost no moisture out. Stop heating and stirring, cool to room temperature, and filter. The obtained 350g filtrate is a crude anthracene solution, and the filter cake is carbazole potassium; the carbazole potassium salt is hydrolyzed, and the product is repeatedly washed with water until pH = 7, and the filter cake is dried to obtain 30g Refined carbazole;

[0022] Step 4. Distill the crude anthracen...

Embodiment 2

[0025] Step 1, the coal tar after the dehydration treatment is distilled at atmospheric pressure, and the fraction between 300 and 360 ° C is cut;

[0026] Step 2, cooling all the fractions obtained in the step to room temperature, standing at 0°C for 1 hour to crystallize, and obtaining the anthracene-carba mixture;

[0027] Step 3: Take 100 g of the anthracene-carbamate mixture obtained in step 2, add 900 g of ethanol and 100 g of potassium carbonate, and put them together in a reactor connected to a water separator, stir and heat, and heat to reflux to separate water until almost no water comes out. Stop heating and stirring, cool to room temperature, and filter. The obtained 550g filtrate is a crude anthracene solution, and the filter cake is carbazole potassium; the carbazole potassium salt is hydrolyzed, and the product is repeatedly washed with water until pH = 7, and the filter cake is dried to obtain 33g Refined carbazole;

[0028] Step 4. Distill the crude anthracen...

Embodiment 3

[0031] Step 1, the coal tar after the dehydration treatment is distilled at atmospheric pressure, and the fraction between 300 and 360 ° C is cut;

[0032] Step 2, cooling all the fractions obtained in the step to room temperature, standing for crystallization at 5°C for 3 hours, and obtaining an anthracene-carba mixture;

[0033] Step 3: Take 100 g of the anthracene-carbamate mixture obtained in Step 2, add 500 g of ether and 100 g of potassium bicarbonate, and put them together into a reactor connected to a water separator, stir and heat, heat and reflux to separate water until almost no water comes out . Stop heating and stirring, cool to room temperature, and filter. The obtained 420g filtrate is crude anthracene solution, and the filter cake is carbazole potassium; the carbazole potassium salt is hydrolyzed, and the product is washed repeatedly with water until pH=7, and the filter cake is dried to obtain 28g Refined carbazole;

[0034] Step 4. Distill the crude anthrac...

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Abstract

The invention relates to a method for preparing refined anthracene by using coal tar as a raw material, which belongs to the technical field of coal tar chemical industry. The method comprises the following steps of distilling the dewatered coal tar under a normal pressure, cutting and fetching fractions between 300 DEG C and 360 DEG C, carrying out freezing crystallization to obtain an anthracene-carbazole mixture, then carrying out chemical separation to obtain semi-refined anthracene, and carrying out sublimation recrystallization to obtain the refined anthracene. In the method, a solvent and a crystallization method are combined, so that carbazole can also be obtained while the refined anthracene is prepared, the usage amount of the solvent is small, the yield of products is high, a filtrate can be recycled, and the pollution to environment is small.

Description

technical field [0001] The invention relates to a method for preparing refined anthracene by using coal tar as a raw material, and belongs to the technical field of coal tar chemical industry. Background technique [0002] Coal tar is one of the products in the crude gas generated by coal pyrolysis in coking industry. It is mainly composed of polycyclic aromatic compounds, with less alkylaromatic content, more high boiling point components, and good thermal stability. More than 500 compounds have been identified, accounting for about 55% of the total coal tar. [0003] The crude anthracene obtained from coal tar contains 25% to 40% of anthracene and 10% to 18% of carbazole. The extraction methods of refined anthracene and carbazole mainly include solvent washing method (Guo Penghui, Hao Juanjuan. Progress in separation technology of anthracene, phenanthrene and carbazole in coal tar[J]. Hebei Chemical Industry, 2008, 31(11): 17-20.) and Combination of distillation and crys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C15/28C07C7/04C07C7/14C07C7/00
Inventor 韩钊武
Owner 韩钊武
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