A kind of preparation method of high-purity 1-methylnaphthalene
A methylnaphthalene, high-purity technology, applied in chemical instruments and methods, purification/separation of hydrocarbons, organic chemistry, etc., can solve problems such as low extraction rate and waste of raw materials, and achieve the effect of improving purity
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[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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