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A method for continuously preparing diacetyl using a reactive distillation tower

The technology of a reactive distillation column and a distillation column is applied in the field of flavor and fragrance production, and can solve the problems of difficulty in large-scale production, large environmental pollution of waste acid, expensive catalyst, etc., and achieve the effects of prolonging the service life and reducing the amount of production.

Active Publication Date: 2021-07-20
YANCHENG CITY CHUNZHU AROMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Methyl ethyl ketone (butanone) oxidation synthesis method, the method uses selenium dioxide ozonation, uses Co 3 o 4 , NiO and other alkali metal catalyzed oxidation methods, nitrite oxidation methods, etc. These methods have the problems of expensive catalysts, difficult preparation of catalysts, and large environmental pollution such as waste acid produced by the production process, which is difficult to achieve large-scale production.

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  • A method for continuously preparing diacetyl using a reactive distillation tower
  • A method for continuously preparing diacetyl using a reactive distillation tower

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Example 1: Continuous preparation of 2,3-butanedione using a reactive distillation column

[0082] This embodiment uses the attached figure 1 The described reactive distillation scheme was implemented.

[0083] The steps of this diacetyl preparation method are as follows:

[0084] A. The reaction of acetoin with ferric chloride

[0085] Under normal pressure, acetoin is added dropwise in the reaction section (1) of rectifying tower still by the first feeding tank (5), simultaneously adds ferric chloride by ferric chloride feed port (8), and acetoin The molar ratio to ferric chloride is 1:0.14;

[0086] Under the agitation of stirring speed 80pm, this reaction mixture is heated to temperature 124 ℃ and carries out reactive rectification, and the temperature of tower top condenser (3) is controlled at 40 ℃ simultaneously, when forming total reflux in the whole rectifying column, reflux The ratio R1 is controlled at 10:1;

[0087] B. Add hydrogen peroxide drop by drop...

Embodiment 2

[0095] Example 2: Continuous preparation of 2,3-butanedione using a reactive distillation column

[0096] This embodiment uses the attached figure 1 The described reactive distillation scheme was implemented.

[0097] The steps of this diacetyl preparation method are as follows:

[0098] A. The reaction of acetoin with ferric chloride

[0099] Under normal pressure, acetoin is added dropwise in the reaction section (1) of rectifying tower still by the first feeding tank (5), simultaneously adds ferric chloride by ferric chloride feed port (8), and acetoin The molar ratio to ferric chloride is 1:0.18;

[0100] Under the agitation of stirring speed 80pm, this reaction mixture is heated to temperature 130 ℃ and carries out reactive rectification, and the temperature of tower top condenser (3) is controlled at 50 ℃ simultaneously, when forming total reflux in the whole rectifying column, reflux The ratio R1 is controlled at 6:1;

[0101] B. Add hydrogen peroxide drop by drop ...

Embodiment 3

[0109] Example 3: Continuous preparation of 2,3-butanedione using a reactive distillation column

[0110] This embodiment uses the attached figure 1 The described reactive distillation scheme was implemented.

[0111] The steps of this diacetyl preparation method are as follows:

[0112] A. The reaction of acetoin with ferric chloride

[0113] Under normal pressure, acetoin is added dropwise in the reaction section (1) of rectifying tower still by the first feeding tank (5), simultaneously adds ferric chloride by ferric chloride feed port (8), and acetoin The molar ratio to ferric chloride is 1:0.10;

[0114] Under the agitation of stirring speed 150pm, this reaction mixture is heated to temperature 100 ℃ and carries out reactive rectification, and the temperature of tower top condenser (3) is controlled at 60 ℃ simultaneously, when forming total reflux in the whole rectifying column, reflux The ratio R1 is controlled at 2:1;

[0115] B. Add hydrogen peroxide drop by drop...

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Abstract

The invention relates to a method for continuously preparing diacetyl by using a reactive distillation tower. The preparation method comprises the steps of reacting acetoin and ferric chloride, adding hydrogen peroxide dropwise, adjusting the reflux ratio, supplementing acetoin and hydrogen peroxide, and the like. The present invention adopts the reactive distillation method to realize the continuous production of 2,3-butanedione products, and the purity of the prepared 2,3-butanedione products reaches more than 99%; The amount of ferric chloride is greatly reduced, and the Fe content of ferric chloride 3+ is reduced to Fe when participating in the oxidation of acetoin as an oxidizing agent 2+ , the hydrogen peroxide will again Fe 2+ Fe oxide 3+ , which prolongs the service life of ferric chloride, achieves the effect of repeated recycling, and greatly reduces the generation of solid waste. The method of the invention is an environmentally friendly synthesis process route.

Description

【Technical field】 [0001] The invention belongs to the technical field of essence and fragrance production. More specifically, the present invention relates to a method for continuously producing diacetyl using a reactive distillation column. 【Background technique】 [0002] 2,3-Butanedione, also known as diacetyl, chemical formula C 4 h 6 o 2 , molecular weight 86.09, CAS431-03-8, creamy aroma. It is mainly used to prepare flavors such as cream, cheese fermented flavor and coffee. It is an edible flavor approved by my country and the world according to GB2760-2014, FEMA2370. In nature, diacetyl widely exists in the essential oils of various plants, such as iris oil, angelica oil, bay oil, etc., and is the main component of butter and some other natural product aromas. [0003] At present, methods for synthesizing 2,3-butanedione include, for example, microbial fermentation. This method uses glucose, starch, etc. as carbon sources, and uses specific microorganisms to conv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/30C07C45/82C07C49/12
CPCC07C45/30C07C45/82C07C49/12Y02P20/10
Inventor 王冠李维虎
Owner YANCHENG CITY CHUNZHU AROMA