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Method for concentrating and separating low-level anthracene and carbazole in residue after extraction of anthracene and carbazole

A low content, carbazole technology, applied in the field of extraction, can solve the problems of no economic value, low efficiency, high separation cost, etc.

Inactive Publication Date: 2010-08-25
JIANGDU RUNHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the solvent method is still used to separate these low mass fractions of anthracene and carbazole, due to the rules of dissolution and crystallization equilibrium, the effect is low efficiency, high separation cost, and no economic value.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Take 1000 g of the residue after extracting anthracene and carbazole, its main composition is 43% phenanthrene, 13% fluorene, 10.6% anthracene, and 8.7% carbazole. Put it into a 2000ml reaction bottle and heat up to 110°C-120°C to melt, then control the temperature at 100°C-110°C, and stir slowly for 2-4 hours. After obvious crystals appear, separate the molten liquid while it is hot, and then heat up the crystallization After reaching 120°C-140°C, it is in a molten state, control the temperature at 110°C-120°C, and stir slowly for 2-4 hours. After the crystallization is formed, separate the molten liquid while it is hot, and then raise the temperature of the crystallization to 130°C-150 ℃, after it is in a molten state, control the temperature at 120-130 ℃, and stir slowly for 2-4 hours. After the crystals are formed, separate the molten liquid while it is hot. Repeat this step by step to increase the melting and crystallization temperature to 140-150 ℃ to obtain 278 g...

Embodiment 2

[0011] Take 1000 g of the residue after extracting anthracene and carbazole, its main composition is 41% phenanthrene, 13% fluorene, 11.6% anthracene, and 9.7% carbazole. Put it into a 2000ml reaction bottle and heat up to 110°C-120°C to melt, then control the temperature at 100°C-110°C, and stir slowly for 2-4 hours. After obvious crystals appear, separate the molten liquid while it is hot, and then heat up the crystallization After reaching 120°C-140°C, it is in a molten state, control the temperature at 110°C-120°C, and stir slowly for 2-4 hours. After the crystallization is formed, separate the molten liquid while it is hot, and then raise the temperature of the crystallization to 130°C-150 ℃, after it is in a molten state, control the temperature at 120-130 ℃, and stir slowly for 2-4 hours. After the crystals are formed, separate the molten liquid while it is hot. 290 g of crystals were obtained, and analyzed by gas chromatography, the anthracene content was 32%, and the ...

Embodiment 3

[0013] Take 1000 g of the residue after extracting anthracene and carbazole, its main composition is 43% phenanthrene, 13% fluorene, 10.6% anthracene, and 8.7% carbazole. Put it into a 2000ml reaction bottle and heat up to 110°C to 120°C to melt, then control the temperature at 100°C to 110°C, and stir slowly for 2 to 4 hours. 120°C~140°C, after it is in a molten state, control the temperature at 110°C~120°C. Stir slowly for 2~4 hours. After the crystals are formed, separate the molten liquid while it is hot, and then raise the temperature of the crystals to 130°C~150°C , after being molten, control the temperature at 120-130°C, and stir slowly for 2-4 hours. After the crystals are formed, separate the molten liquid while it is hot. Repeat this step by step to increase the melting and crystallization temperature to 170-180°C to obtain 220 grams of crystals were analyzed by gas chromatography, and the anthracene content was 38%, and the carbazole content was 29%. The anthracen...

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Abstract

The invention discloses a method for concentrating and separating low-level anthracene and carbazole in residue after the extraction of anthracene and carbazole and relates to the technical field of an extraction method. The method comprises the following steps: using a plurality of melt crystallization separation tanks to escalate the melt crystallization temperature from 100 DEG C to 180 DEG C, and separating low-melting point components step by step to obtain high-melting point crystals with high mass fraction of anthracene and carbazole. The invention utilizes the characteristic of large melting point difference of the above substances and adopts the zone melting and multi-level melting methods to separate low-melting point substances step by step, obtain high-melting point substances and ensure that low-level anthracene and carbazole in the original residue to be collected in the high-melting point substance area; and in the high-melting point substance area, the content of anthracene can be increased to 30-35wt%, and the content of carbazole can be increased to 25-30wt%. The high-melting point substances can be continuously purified through conventional solvent method, and the purities of anthracene and carbazole can be continuously increased through multi-level melting separation to obtain anthracene and carbazole products with high mass fractions.

Description

technical field [0001] The invention relates to the technical field of extraction methods, in particular to a method for concentrating and separating residual low-content anthracene and carbazole in the residue after extracting anthracene and carbazole. Background technique [0002] Anthracene and carbazole are important raw materials for the production of dyes, pigments and pharmaceutical products. At present, most domestic enterprises use crude anthracene, the separation product of coal tar, as raw materials to obtain high-purity anthracene (more than 90% content) and carbazole (more than 93% content) through solvent extraction and separation. The residue after azole is usually used as fuel or carbon black is fired or concrete water reducer is made, because in the process of solvent extraction, it is repeatedly separated by dissolution-supersaturated crystallization method to improve the purity of the target product. After the dissolution and crystallization are balanced,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C15/28C07C7/14C07D209/86C07D209/84
Inventor 徐兆桐
Owner JIANGDU RUNHUA CHEM
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