Preparation method of high-purity 1-methylnaphthalene

A methyl naphthalene, high-purity technology, used in chemical instruments and methods, hydrocarbon purification/separation, hydrocarbons, etc., can solve the problems of low extraction rate, waste of raw materials, etc., and achieve the effect of improving purity

Active Publication Date: 2017-07-21
PENG CHEN NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the extraction of α-methylnaphthalene and β-methylnaphthalene from industrial methylnaphthalene fractions mainly adopts the methods of distillation, crystallization and suction filtration, that is, the industrial methylnaphthalene fractions are directly immersed in a rectification tower for rectification. Product purity, according to the different crystallization points of α-methylnaphthalene and β-methylnaphthalene, is purified in the crystallizer. This process has the defects of waste of raw materials and low extraction rate

Method used

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preparation example Construction

[0018] The preparation method of the high-purity 1-methylnaphthalene of the present invention comprises the following steps: (a) adding industrial methylnaphthalene fractions into an acidic solution for pickling, standing and stratifying to obtain the first organic layer; (b) The first organic layer is added to an alkaline solution for alkali washing, and the second organic layer is obtained by standing and layering; (c) adding ethanethiol, metal halides and catalysts to the second organic layer for reflux reaction; The mass ratio of the second organic layer, ethanethiol, metal halide and catalyst is 100:80~150:1~5:0.5~2; the catalyst is a mixture of copper oxide and aluminum oxide, and its mass ratio is 1: 1~3; (d) The product of step (c) can be filtered and rectified. The industrial methylnaphthalene distillate is acid-washed and alkali-washed successively, and reflux reaction is carried out in ethanethiol, metal halide and catalyst, so that the selective removal of 2-methyl...

Embodiment 1

[0022] The present embodiment provides a kind of preparation method of high-purity 1-methylnaphthalene, it comprises the following steps:

[0023] (a) Add industrial methylnaphthalene fractions (mainly containing 1-methylnaphthalene, 2-methylnaphthalene, quinoline and indole) to a sulfuric acid solution with an excess mass concentration of 10% (usually industrial methylnaphthalene and its volume ratio are 1:5~10), pickling at 40°C, standing for stratification, discarding the water layer to obtain the first organic layer;

[0024] (b) Add the organic layer to a sodium bicarbonate solution with a mass concentration of 5% for alkali washing at 70°C to make it close to neutral (the test paper does not change color), let it stand for layers, and discard the water layer to obtain the second Two organic layers;

[0025] (c) Add ethanethiol, metal halide and catalyst to the second organic layer for reflux reaction (reflux temperature is about 40°C); the mass ratio of the second organ...

Embodiment 2

[0028] The present embodiment provides a kind of preparation method of high-purity 1-methylnaphthalene, it comprises the following steps:

[0029] (a) Add industrial methylnaphthalene fractions (mainly containing 1-methylnaphthalene, 2-methylnaphthalene, quinoline and indole) to a sulfuric acid solution with an excess mass concentration of 30% (usually industrial methylnaphthalene and its volume ratio are 1: 1~3), carry out pickling under the condition of 60 ℃, let stand for stratification, discard the water layer to get the first organic layer;

[0030] (b) Add the organic layer to a sodium bicarbonate solution with a mass concentration of 10% for alkali washing at 90°C to make it close to neutral (the test paper does not change color), let it stand for layers, and discard the water layer to obtain the second Two organic layers;

[0031] (c) Add ethanethiol, metal halide and catalyst to the second organic layer for reflux reaction (reflux temperature is about 40°C); the mass...

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Abstract

The invention relates to a preparation method of high-purity 1-methylnaphthalene. The preparation method comprises the steps that (a) technical methylnaphthalene fraction is added to an acid solution for acid pickling, and standing layering is performed to obtain a first organic layer; (b) the first organic layer is added to an alkaline solution for alkaline washing, and standing layering is performed to obtain a second organic layer; (c) ethanethiol, metal halide and a catalyst are added to the second organic layer for reflux reaction; the mass ratio of the second organic layer, the ethanethiol, the metal halide and the catalyst is 100:(80-150):(1-5):(0.5-2); the catalyst is a mixture of copper oxide and aluminium trioxide, and the mass ratio of the copper oxide and the aluminium trioxide is 1:(1-3); (d) the product of the step (3) is filtered and rectified so that the high-purity 1-methylnaphthalene is obtained. Accordingly, 2-methylnaphthalene can be selectively removed, and the purity of the 1-methylnaphthalene is improved greatly.

Description

technical field [0001] The invention relates to a preparation method of oil agent methylnaphthalene, in particular to a preparation method of high-purity 1-methylnaphthalene. Background technique [0002] 1-Methylnaphthalene (that is, α-methylnaphthalene) is a colorless oily liquid with a naphthalene-like odor that can volatilize with steam. It is flammable, insoluble in water, and easily soluble in ether and ethanol; its relative density (20°C) 1.025, boiling point 245°C and flash point 82.2°C. Methylnaphthalene is the main raw material for the production of disperse dye auxiliaries (dispersants). It can also be used as a heat carrier and solvent, a surfactant, a sulfur extraction agent, and can also be used to produce plasticizers and fiber dyeing aids. It can also be used to determine alkane value and cetane number of standard fuels. [0003] At present, the extraction of α-methylnaphthalene and β-methylnaphthalene from industrial methylnaphthalene fractions mainly adop...

Claims

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Application Information

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IPC IPC(8): C07C7/00C07C15/24
CPCC07C7/005C07C15/24
Inventor 谈勇谈俊江晓龙乔久昌张惠根
Owner PENG CHEN NEW MATERIALS TECH CO LTD
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