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Catalyst for preparing glyoxal by oxidizing acetaldehyde and preparation method thereof

A technology of catalyst and glyoxal, which is applied in the field of chemical technology, can solve problems such as unseen industrial application, poor economy of glyoxal, and environmental pollution, so as to improve the economic benefits and market competitiveness of enterprises, avoid easy pollution of the environment, and produce products high quality effect

Active Publication Date: 2012-02-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there has been no follow-up report since then, let alone industrial application
Although pure selenium dioxide is prepared as oxidant oxidation acetaldehyde and glyoxal has higher selectivity and glyoxal yield, selenium dioxide is comparatively expensive, and production glyoxal economy is relatively poor; And selenium dioxide oxidation acetaldehyde After the reaction, selenium dioxide is reduced to elemental selenium and becomes precipitated. If it is not recycled, it will pollute the environment

Method used

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  • Catalyst for preparing glyoxal by oxidizing acetaldehyde and preparation method thereof
  • Catalyst for preparing glyoxal by oxidizing acetaldehyde and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A, take by weighing 2g FX-II type modified zeolite, be that 10% selenous acid solution with 50 milliliters of mass percent concentrations fully stir 3 hours, vacuum dry 3 hours under 60 ℃, selenium dioxide (wt%) and FX - The ratio of type II modified zeolite (wt%) is 0.1:1.

[0021] B, 10g (mass fraction is 40%) acetaldehyde solution and the catalyzer that 0.25g step A make add in the 250 milliliter reactor that reflux condenser, agitator and thermometer are housed, stir, and control reaction temperature is 70 ± 2 ℃, add hydrogen peroxide dropwise, the molar ratio of hydrogen peroxide to acetaldehyde is 0.25:1, the time for adding hydrogen peroxide is 2 hours, after 2.5 hours of reaction, let it stand still, and filter out the carrier from the reaction solution. The yield of glyoxal was analyzed to be 6.45%, and the selectivity of acetaldehyde was 93.47%.

Embodiment 2

[0023] A, take by weighing the gac of 2g, be that 10% selenous acid solution of 50 milliliters of mass percent concentrations fully stir 3 hours, vacuum-dry 3 hours at 60 ℃, selenium dioxide (wt%) and gac (wt%) ) ratio is 0.2:1.

[0024] B, 10g (mass fraction is 40%) acetaldehyde solution and the catalyzer that 0.5g step A make add in the 250 milliliter reactor that reflux condenser, agitator and thermometer are housed, stir, and control reaction temperature is 50 ± 2 ℃, add hydrogen peroxide dropwise, the molar ratio of hydrogen peroxide to acetaldehyde is 1.25:1, the time for adding hydrogen peroxide is 2 hours, after 2.5 hours of reaction, let it stand still, and filter out the carrier from the reaction solution. The yield of glyoxal was analyzed to be 46.45%, and the selectivity of acetaldehyde was 83.87%.

Embodiment 3

[0026] A, take by weighing 2g polystyrene, add 50 milliliters of mass percent concentrations and be in the selenous acid solution of 15%, fully stir 3 hours, vacuum-dry 3 hours at 50 ℃, selenium dioxide (wt%) and polystyrene The ratio of ethylene (wt%) was 0.2:1.

[0027] B, 10g (mass fraction is 40%) acetaldehyde solution and 0.5g step A make catalyst and add in the 250 milliliter reactor that reflux condenser, stirrer and thermometer are housed, stir, and control reaction temperature is 50 ± 2 ℃ , add hydrogen peroxide dropwise, the molar ratio of hydrogen peroxide to acetaldehyde is 3:1, the time for adding hydrogen peroxide is 2 hours, after reacting for 3 hours, let it stand still, and filter out the carrier from the reaction solution. The yield of glyoxal is 35.52%, and the selectivity of glyoxal is 70.36%.

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Abstract

The invention relates to a catalyst for preparing glyoxal prepared from aldehyde and a preparation method thereof. The preparation method comprises the following steps: dissolving selenium dioxide inwater to prepare a selenious acid solution with the mass percentage of 5-40% , adding a proper amount of carrier into the selenious acid solution, sufficiently stirring for 1-6 hours, drying for 3-5 hours at 40-70 DEG C in vacuum to prepare a load selenium dioxide catalyst in which the mass ratio of the selenium dioxide to the carrier is 0.02-0.05:1; or uniformly mixing and stirring the selenium and the carrier with the mass ratio of 0.05-1:1 and screening to prepare a load selenium catalyst. For preparing the aldehyde, the mass ratio of the catalyst to the aldehyde is 0.025-0.5:1, hydrogen peroxide is used as an oxidant, the molar ratio of the hydrogen peroxide to the aldehyde is 0.25-5:1, and a reaction is carried out for 0.5-5 hours at 25-85 DEG C; under the optimization condition, theyield of the glyoxal is larger than 30%, and the selectivity is over 80%. The preparation method of the glyoxal has mild reaction condition, higher selectivity and yield and better industrial application prospect.

Description

technical field [0001] The invention relates to a catalyst for oxidizing acetaldehyde to prepare glyoxal and a preparation method thereof, in particular to a method for preparing a catalyst containing selenium or selenium dioxide and its application in the process of oxidizing acetaldehyde to prepare glyoxal. The invention belongs to the technical field of chemical technology in the chemical industry. Background technique [0002] Glyoxal, also known as oxalic acid aldehyde, is the simplest α-dicarbonyl compound. In addition to the generality of aliphatic aldehydes, its molecule contains two interconnected carbonyl groups and has some special chemical properties. Addition or condensation reaction with alcohols, amines, amides, aldehydes and hydroxyl-containing compounds, etc., and cross-linking reactions with proteinaceous animal glue, cellulose, polyvinyl alcohol and urea, etc., is a very versatile Chemical raw materials and intermediates are widely used in papermaking, te...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/057C07C45/28C07C47/127B01J31/06B01J31/02B01J29/70
CPCY02P20/584
Inventor 姚小利崔群李晓强王海燕陈新华朱鸭梅
Owner CHINA PETROLEUM & CHEM CORP