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Method for preparing beta-methyl naphthoquinone through catalytic oxidation of beta-methylnaphthalene by MCM-41 molecular sieve with iron-containing framework

A MCM-41, catalytic oxidation technology, applied in the preparation of oxidized quinone, organic chemistry, etc., can solve the problems of high economic cost, high production cost, expensive cerium salt and power consumption, etc.

Inactive Publication Date: 2011-11-23
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because cerium salt is very expensive and the power consumption during oxidation is too large, the economic cost is too high, and it is difficult to use it widely.
Zhu Ai Shi and others (Zhu Ai Shi, Sun Jun. Chinese Journal of Pharmaceutical Industry . 1999,30,324) with organic peroxides (such as peracetic acid) as oxidants, glacial acetic acid as reaction medium, the reaction to obtain β-menaquinone products with a mass fraction of 98%, but because some organic peroxides are relatively Expensive, so the production cost of this method is higher

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0012] The following examples are only used to specifically illustrate the present invention. But the scope of protection of the present invention is not limited to the following examples. (The following is the mass percentage content) Example 1: Put 0.05g of Fe-MCM-41 catalyst (4% iron content), 0.5g of β-methylnaphthalene, and 14g of acetonitrile into the reactor, mix and stir evenly, and continue to stir The temperature was raised to 100° C., and 3 g of hydrogen peroxide was added slowly, and the addition was completed in 15 minutes. After reacting for 1 hour, the mixture was filtered and separated to obtain the product β-menaquinone. Gas chromatography analysis: the conversion rate of β-methylnaphthalene is 61%, and the selectivity of β-menaphthoquinone is 35%.

Embodiment 2

[0013] Example 2: Put 0.1g of Fe-MCM-41 catalyst (iron content 25%), 0.5g of β-methylnaphthalene, and 14g of acetonitrile into the reaction kettle, mix and stir evenly, heat up to 100°C under continuous stirring conditions, and slowly add 3 g of hydrogen peroxide was added over 15 minutes. After reacting for 1 hour, the mixture was filtered and separated to obtain the product β-menaquinone. Gas chromatography analysis: the conversion rate of β-methylnaphthalene is 71%, and the selectivity of β-menaphthoquinone is 31%.

Embodiment 3

[0014] Example 3: Put 0.05g of Fe-MCM-41 catalyst (8% iron content), 0.5g of β-methylnaphthalene, and 14g of acetonitrile into the reaction kettle, mix and stir evenly, heat up to 100°C under continuous stirring conditions, and slowly add 3 g of hydrogen peroxide was added over 15 minutes. After reacting for 1 hour, the mixture was filtered and separated to obtain the product β-menaquinone. Gas chromatography analysis: the conversion rate of β-methylnaphthalene is 65%, and the selectivity of β-menaphthoquinone is 36%.

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Abstract

The invention relates to a method for preparing beta-methyl naphthoquinone through catalytic oxidation of beta-methylnaphthalene by an MCM-41 molecular sieve with an iron-containing framework. Specifically, an MCM-41 molecular sieve with an iron-containing framework is employed as a catalyst to oxidize beta-methylnaphthalene for preparing beta-methyl naphthoquinone, with a beta-methylnaphthalene conversion rate of 65% and a beta-methyl naphthoquinone selectivity of 37%. The method of the invention can substantially improve the conversion rate in beta-methyl naphthoquinone production through beta-methylnaphthalene oxidation, and greatly shorten the reaction time. Wherein, the catalyst is repeatedly usable.

Description

technical field [0001] The invention relates to a preparation method of β-menaquinone, and relates to an MCM-41 molecular sieve catalyst whose skeleton contains iron. Background technique [0002] β-menaquinone is an important intermediate in the synthesis of K-series vitamins, and is widely used in medicine and feed additives. Due to the wide application of β-menaquinone, there are many literatures reporting the synthesis method of this compound. [0003] Nakaoji K et al. reported in their patent (Nakaoji Kozo, Nakaoji Shigeru. JP:10245358, 1998.) that dichromic acid was used to treat β-menaquinone aqueous solution at 90°C for about 2.7 hours, and the yield could reach 64.7 %. This process will produce a large amount of chromium-containing wastewater in the production process, which is complicated and difficult to deal with and seriously pollutes the environment. Yamaguchi S, et al (Yamaguchi S, Inoue M. J. Chem Pharm Bull . 1986,34,445) reported the method of oxidizing...

Claims

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Application Information

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IPC IPC(8): C07C50/10C07C46/04
Inventor 范以宁裘婧陈泱庄柯
Owner NANJING UNIV
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