Method for enriching thianaphthene from mixtures containing thianaphthene and naphthalene

A technology of mixture and thiane, applied in the direction of organic chemistry, can solve the problem of insufficient enrichment efficiency of thiane

Active Publication Date: 2010-06-23
BAOWU CHARCOAL MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Separation of thianthene and naphthalene by solvent crystallization is currently only used for the purification of naphthalene, and there is no report for the enrichment of thianthene
In addition, commonly used monohydric alcohol solvents are not efficient enough for the enrichment of thioindenes

Method used

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  • Method for enriching thianaphthene from mixtures containing thianaphthene and naphthalene
  • Method for enriching thianaphthene from mixtures containing thianaphthene and naphthalene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dissolve 200 grams of refined naphthalene crystallization residual oil containing 8.08% of thioindenes and 71.16% of naphthalene in 200 grams of 1,3-butanediol at 60° C., and stir to form a solution. The solution is then naturally cooled to 20°C to crystallize naphthalene and other impurities. Then, the solution is filtered to separate crystals obtained by crystallization, and the obtained filtrate is crystallization mother liquor. Finally, the crystallization mother liquor was distilled to 215° C. to separate 1,3-butanediol to obtain 32.23 g of enriched thiabene fractions. The content of thiabene was 20.18% according to gas chromatography. Obviously, thiabene was effectively enriched.

[0021] (The naphthalene fraction obtained after the distillation of coal tar is industrial naphthalene. Industrial naphthalene is melted and crystallized step by step to prepare a refined naphthalene product with a naphthalene content of more than 99%, and the rest is the refined naphth...

Embodiment 2

[0026] Dissolve 200 grams of refined naphthalene crystallization residual oil containing 8.08% of thioindenes and 71.16% of naphthalene in 400 grams of 1,3-butanediol at 60° C., and stir to form a solution. The solution is then naturally cooled to 20°C to crystallize naphthalene and other impurities. Then, the solution is filtered to separate crystals obtained by crystallization, and the obtained filtrate is crystallization mother liquor. Finally, the crystallization mother liquor was distilled to 215° C. to separate 1,3-butanediol to obtain 46.73 g of enriched thiabene fractions. The thiabene content was 18.06% according to gas chromatography, obviously thiabene was effectively enriched.

[0027] Comparative experiment 2:

[0028] Dissolve 200 grams of refined naphthalene crystallization residual oil containing 8.08% of thioindenes and 71.16% of naphthalene in 400 grams of ethanol at 60° C., and stir to form a solution. Then the solution was naturally cooled to 20°C to crys...

Embodiment 3

[0031] Dissolve 200 grams of refined naphthalene crystallization residual oil containing 8.08% of thioindenes and 71.16% of naphthalene in 100 grams of 1,3-butanediol at 65° C., and stir to form a solution. The solution is then naturally cooled to 20°C to crystallize naphthalene and other impurities. Then, the solution is filtered to separate crystals obtained by crystallization, and the obtained filtrate is crystallization mother liquor. Finally, the crystallization mother liquor was distilled to 215° C. to separate 1,3-butanediol to obtain 18.54 g of enriched thiabene fractions. According to gas chromatography analysis, the thiabene content was 24.43%. Obviously, thiabene was effectively enriched.

[0032] Comparative experiment 3:

[0033] Dissolve 200 grams of refined naphthalene crystallization residual oil containing 8.08% of thioindenes and 71.16% of naphthalene in 100 grams of ethanol at 65° C., and stir to form a solution. Then the solution was naturally cooled to 2...

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Abstract

The invention relates to a thianaphthene-enriching method, in particular to a method for enriching thianaphthene from mixtures containing thianaphthene and naphthalene, specifically a method for enriching thianaphthene from coal-tar downstream products. The method comprises the following: a) a step of dissolving, which is to dissolve a mixture containing thianaphthene and naphthalene in binary alcohol serving as solvent and form solution at 60 to 80 DEG C; b) a step of crystallizing, which is to cool the solution obtained in a step a) to room temperature and crystallize naphthalene and other impurities from the solution obtained in the step a); c) a step of filtering, which is to filter and separate the naphthalene and the other impure crystals and obtain crystallization mother liquor; and d) a step of distilling, which is to distill the crystallization mother liquor to remove the binary alcohol and obtain enriched thianaphthene fractions. Different from the prior naphthalene solvent crystallization adopting the monohydric alcohol as solvent in general, the method significantly raises the enrichment degree of thianaphthene by adopting the binary alcohol as the solvent.

Description

technical field [0001] The invention relates to a method for enriching thianthene, in particular to a method for enriching thianthene from a mixture containing thianthene and naphthalene, in particular to a method for enriching thianthene from downstream products of coal tar. Background technique [0002] Thianthene, also known as benzothiophene, is an important fine chemical raw material widely used in medicine, pesticides, optical materials and dyes. The mass fraction of thianthene in coal tar is about 0.4%, and the thianthene resource in coal tar is mainly concentrated in the naphthalene fraction after coal tar distillation, and the naphthalene crystallization residue contains about 10% thianthene. Currently, there are be fully utilized. [0003] Thianthene and naphthalene have similar boiling points, and it is very difficult to separate them by ordinary rectification. According to the characteristic that thioindenes and naphthalene have different solubility in solvent,...

Claims

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Application Information

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IPC IPC(8): C07D333/54
Inventor 王仁远王焕煜
Owner BAOWU CHARCOAL MATERIAL TECH CO LTD
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