Method for preparing butanedione through oxidating acetylmethylcarbinol

A technology of acetoin and diacetyl, applied in the field of oxidation of acetoin to diacetyl, can solve the problems of high production cost, rare raw materials, difficult purification of products, etc., and achieve low production cost, simple operation and high selectivity Effect

Inactive Publication Date: 2005-10-26
DALIAN LAIKE FINE CHEM CO LTD
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Problems solved by technology

This method has a large amount of wastewater, the product is difficult to purify, and the production cost is high
Later, some people used the 2,3-butanediol method obtained by hydrolysis or fermentation as raw material to synthesize diacetyl through catalytic dehydrogenation, but because the raw material is rare, it is ...

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  • Method for preparing butanedione through oxidating acetylmethylcarbinol

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Embodiment Construction

[0012] The present invention will be further described in detail below in combination with the technical scheme and the best embodiment.

[0013] Add 220 g (2.5 mol) of acetoin, 500 ml of water and 1360 g of hexahydrate crystalline ferric chloride (5.0 mol) in a 3-liter three-necked flask equipped with mechanical stirring, dropping funnel, fractionating column and condenser. The mixture was heated to 100°C, and diacetyl was collected until there was no distillate. The water layer of the distillate was removed, and the oil layer was dried with calcium chloride and rectified to obtain 161 grams of diacetyl. The purity of the product is not less than 99%, the refractive index is 1.3935, the boiling point is 88.0-88.5°C, and the yield is 75%.

[0014] Pour the still liquid ferrous chloride into the filter tank to filter. The sieve plate in the middle of the filter tank must be paved with small stones and sand, and then covered with filter cloth. The bottom of the tank should be ...

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Abstract

The present invention relates to a new method for preparing butanedione by utilizing acetoin. Said invention uses acetoin as raw material, and utilizes iron trichloride to produce chemical oxidation so as to obtain butanedione, then make sit undego the process of simple treatment, so that the pure butanedione product whose purity can be up to 99% can be obtained. The oxidant iron trichloride can be converted into iron dichloride, said iron dichloride can be oxidated by nitric acid, and can be reformed into iron trichloride, after the iron trichloride is concentrated, it can be circularly used.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals and relates to a new method for preparing diacetyl by oxidation of acetoin. Background technique [0002] Diacetyl is an important spice and an intermediate in organic synthesis, which can be used in the preparation of flavors and the preparation of heterocyclic compounds. At present, the method for synthesizing diacetyl is to use methyl ethyl ketone as raw material, and prepare diacetyl through nitrosation reaction. This method has a large amount of wastewater, the product is difficult to purify, and the production cost is high. Later, someone used 2,3-butanediol obtained by hydrolysis or fermentation as a raw material to synthesize diacetyl through catalytic dehydrogenation, but the raw material was difficult to obtain industrially. [0003] In addition, isobutanol is used as a raw material to produce diacetyl through catalytic oxidation rearrangement (Chinese patent application number:...

Claims

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Application Information

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IPC IPC(8): C07C49/12
Inventor 王之建孙芝贾卫民
Owner DALIAN LAIKE FINE CHEM CO LTD
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