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

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

CN102746103AInactive Publication Date: 2012-10-24韩钊武

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

Patent Timeline
24 Oct 2012
Publication
CN102746103A
IPC
C07C15/28; C07C7/04; C07C7/14; C07C7/00
Inventors
韩钊武