Alpha-methylnaphthalene purifying technique

A technology of methylnaphthalene and a purification method, which is applied in the technical field of purifying α-methylnaphthalene, can solve problems such as the difficulty in achieving the purity of α-methylnaphthalene, complex components and difficult raw material purification, and achieve low price and high product quality. The effect of good quality and wide range of solvent sources

Active Publication Date: 2008-09-24
BAOWU CHARCOAL MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The method introduced in the above-mentioned literature only has a better removal effect on nitrogen-containing impurities such as indole in the α-methylnaphthalene fraction, but the removal of sulfur-containing impurities such as methylthianaphthene is not thorough, so α- The purity of methylnaphthalene is difficult to reach more than 99%
[0004] The present inventor considers that the α-methylnaphthalene raw material composition composition component that removes indole is complex (containing β-methylnaphthalene, 2-methylthiane, 5-methylthiane, 3-methylthiane and a small amount unknown substance), and because the melting point of α-methylnaphthalene is low, it is liquid at normal temperature, and the content of each impurity in the raw material is low, so it is difficult to purify the raw material by conventional crystallization methods; and because some impurities and α-methylnaphthalene The boiling points of the base naphthalenes are similar, and some may form azeotropes, so it is difficult to obtain high-purity α-methylnaphthalene simply by conventional distillation methods

Method used

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  • Alpha-methylnaphthalene purifying technique
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  • Alpha-methylnaphthalene purifying technique

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The α-methylnaphthalene raw material (composition sees Table 1) that 50g purity is 97.26% of indole joins in the 100ml Erlenmeyer flask, puts into magnetic stirrer, adds powdered anhydrous aluminum trichloride (raw material weight 1.14%), fully stirred, after reacting for 3.5 hours, the solid was filtered off, and the filtrate was taken for analysis. The results are shown in Table 2. In the filtrate, 50 g of dehydrated alcohol (solvent: filtrate ≈ 1: 1) was added to the filtrate. ), transferred to the separatory funnel after fully oscillating, left to stand for 25 minutes, and the upper layer liquid was taken for analysis, the results are shown in Table 3.

[0033] Quantitative analysis of the product was carried out on a Shimadzu GC-2010 gas chromatograph. The chromatographic column was a DB-WAX capillary column with a length of 30 m, an inner diameter of 0.25 mm, and a film thickness of 0.25 μm.

[0034] Table 1 removes the α-methylnaphthalene raw material composition...

Embodiment 2

[0041] The α-methylnaphthalene raw material (composition is shown in Table 1) that 50g purity is 97.26% to remove indole joins in the 100ml Erlenmeyer flask, puts into magnetic stirrer, adds powdery anhydrous aluminum trichloride (raw material 1.45% of the weight), fully stirred, after reacting for 5 hours, filter out the solid in the α-methylnaphthalene, get the filtrate and analyze, the results are shown in Table 4, add heated 42 ℃ dehydrated alcohol 90g in the filtrate (solvent: filtrate ≈ 1.8: 1), after fully oscillating, transfer it to a separatory funnel, let it stand for 30 minutes, get the upper layer liquid for analysis, the results are shown in Table 5, after the upper layer liquid is distilled off to remove the solvent, α-formazan The base naphthalene product weighs 44.8g, and the analytical results of the product are shown in Table 6.

[0042] Quantitative analysis of the product was carried out on a Shimadzu GC-2010 gas chromatograph. The chromatographic column wa...

Embodiment 3

[0050] The α-methylnaphthalene raw material (see Table 1 for composition) that 40g purity is removed indole joins in the 100ml Erlenmeyer flask, puts into magnetic stirrer, adds powdered anhydrous zinc chloride (raw material weight 1.73%), fully stirred, after reacting for 6.5 hours, filter out the solid in the α-methylnaphthalene, get the filtrate and analyze, the results are shown in Table 7, add heated methanol 80g at 39°C in the filtrate (solvent: Filtrate ≈ 2: 1), after fully oscillating, transfer in the separatory funnel, leave standstill for 40 minutes, get the upper layer liquid and analyze, its result is shown in Table 8, after the upper layer liquid is distilled off solvent, obtains α-methyl naphthalene product , weighing 36.2g, the analytical results of the product are shown in Table 9.

[0051] Quantitative analysis of the product was carried out on a Shimadzu GC-2010 gas chromatograph. The chromatographic column was a DB-WAX capillary column with a length of 30 m, a...

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Abstract

The present invention provides a purification method of alpha-methyl-naphthalene. The method comprises the following steps: the alpha-methyl-naphthalene without indole is used as raw material and reacts with metal halides for 3 to 8 hours; the metal halides are selected from AlX3 and ZnX2; wherein, X is atoms of Cl<-> and Br<->; after solids and flocculates generated in the reaction are removed, washing solvent is added into and mixed with the filtrate; then the mixture is standing for 20 to 40 minutes; the washing solvent is selected from methanol, ethanol, propanol, ether or benzene; after the solvent in the upper solution is steamed, the purified alpha-methyl-naphthalene can be prepared. The purification method eliminates most of methyl benzothiophene impurities and unknown substances in the alpha-methyl-naphthalene so that the purity of the alpha-methyl-naphthalene can reach to 99 percent. The purification method has the advantages of high quality of the product, high added value, broad source of the solvent, low price, low energy consumption and so on. The alpha-methyl-naphthalene that is prepared in the purification method can be used as pharmaceutical intermediates, surfactants of terylene printing carriers, or used on other occasions requiring relatively high-purity alpha-methyl-naphthalene.

Description

technical field [0001] The invention relates to a purification process of α-methylnaphthalene, in particular to a process for purifying α-methylnaphthalene from raw materials containing α-methylnaphthalene from which indole has been removed. Background technique [0002] α-Methylnaphthalene can be used in vinyl chloride fiber and polyester printing and dyeing carrier surfactant, heat carrier, pharmaceutical intermediate, sulfur extraction agent, and can be used in the production of plasticizers and fiber dyeing aids. It can also be used as a cetane number measuring agent for diesel oil, a solvent for pesticides and insecticides, and a solvent for the production of hydrogen peroxide by anthraquinone method. It can also be used to synthesize 1-naphthoic acid as a plant growth hormone, and synthesize 1-naphthoic acid as a raw material for color photographic dyes. [0003] In the existing production and purification technology of α-methylnaphthalene, the patent CN94113628.0 int...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/20C07C7/11C07C7/00C07C15/24
Inventor 郑胜华夏剑忠侯文杰吴恢庆
Owner BAOWU CHARCOAL MATERIAL TECH CO LTD
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