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Production of butanedione from 3-hydroxybutanone by gas-phase oxidation

A hydroxybutanone, gas-phase oxidation technology, applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of severe, high reactor requirements, low reaction yield of butanedione, etc. , to achieve the effect of easy operation and control, cost reduction, safe and reliable reaction temperature

Active Publication Date: 2007-02-21
APPLE FLAVOR & FRAGRANCE GRP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires a reaction temperature of 200°C to 500°C, which is more violent and requires higher requirements on the reactor; the reaction yield of diacetyl is low, only 15% to 16%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1: Preparation of 3-hydroxybutanone fermentation broth:

[0029] Preparation of cell liquid cultures of the Bacillus pumilus XH195 DSM 16187 strain. Pick a ring of Bacillus pumilus XH195 DSM 16187 strain cultured on the slant of solid high-glucose LB medium, inoculate it in a 300ml Erlenmeyer flask containing 50ml of sterilized high-glucose LB medium, and place it on a shaker at 37°C Cultivate at a rotational speed of 180r / min for 24 hours to obtain a cell liquid culture of the Bacillus pumilus XH195 DSM 16187 strain.

[0030] The formula of the above-mentioned high-sugar LB medium is: 1L of distilled water contains: 200g of glucose, 10g of peptone, 5.0g of yeast powder, 10g of NaCl, and sterilized at 121°C for 15min. The solid high-glucose LB medium is based on the above formula by adding 20g / L agar powder.

[0031] The above-mentioned Bacillus pumilus XH195 DSM 16187 strain was used to obtain a mature 3-hydroxybutanone fermentation broth with a glucose fermenta...

Embodiment 2

[0044] Repeat the operation procedure of embodiment 1 step 2, change gac into woody gac, the mol ratio of oxygen and 3-hydroxybutanone is changed into 0.75, the space velocity of mixed gas is changed into 1000h -1 , and the reaction temperature was changed to 130°C.

[0045] The reaction yield of diacetyl reaches 75%.

Embodiment 3

[0047] Repeat the operation steps of Example 1 step 2, change the activated carbon into coal-based activated carbon, change the mol ratio of oxygen to 3-hydroxybutanone into 1.00, and change the space velocity of the mixed gas into 1250h -1 , and the reaction temperature was changed to 140°C.

[0048] The reaction yield of diacetyl reaches 82%.

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PUM

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Abstract

Production of diacetyl by 3-alkyl butanone gas-phase oxidation is carried out by heat vaporizing 3-alkyl butanone fermenting liquor or its preparing liquor to obtain steam, mixing the steam with air with mol ratio=2.5:0.5, inducing the mixed gas into fixed bed reactor with active carbon at air speed:500h-1-2500h-1and temperature:110-190 DEG C, collecting diacetyl at exit of fixed bed reactor by condensing. It is simple, safe and costs low. It has low reaction temperature, higher reaction efficiency and purity and no environmental pollution.

Description

technical field [0001] The invention relates to a method for preparing diacetyl, in particular to a novel method for preparing diacetyl by gas-phase oxidation of 3-hydroxybutanone. Background technique [0002] Diacetyl is a flavoring substance that exists in nature. It is used in food, beverage, candy, feed, essence, etc. with milk flavor. It is also an important chemical raw material, which can be used to prepare certain heterocyclic compounds. As gelatin hardener and photographic binder, etc. In addition, diacetyl has a good antiseptic effect, and can kill many pathogenic bacteria at a concentration of 1g / L. [0003] The commonly used industrial production method of diacetyl is to use methyl ethyl ketone as raw material, react with nitrous acid to form butanone oxime, and then add dilute sulfuric acid to decompose to obtain the finished product. The waste water of this method seriously pollutes the environment, and the production cost is relatively high. [0004] The c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/12C07C45/32
CPCC07C45/39C07C49/12
Inventor 陈洪许平肖梓军杜毅曾义勇张兆斌马清仪魏中浩
Owner APPLE FLAVOR & FRAGRANCE GRP
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