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Method for preparing dihydroxy acetone by selectively oxidizing glycerin with hydrogen peroxide

A technology for oxidizing dihydroxyacetone and glycerin, which is applied in the fields of oxidative preparation of carbonyl compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., which can solve the problems of difficult storage, expensive strains, product separation and purification process cumbersome and other problems, to achieve the effect of easy separation, easy operation and good reusability

Active Publication Date: 2012-05-02
NANJING INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the microbial method for producing dihydroxyacetone, the bacteria are expensive, difficult to store, and the product separation and purification process is cumbersome and the problems existing in the direct catalytic oxidation method. The present invention provides a method for preparing dihydroxyacetone by using hydrogen peroxide to selectively oxidize glycerol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 8.61 kg Mn(NO 3 ) 2 ·6H 2 O and 3.75 kg Al(NO 3 ) 3 9H 2 O was made into 120 L solution with deionized water; 1.06 kg Na 2 CO 3 Prepare 120 L solution with deionized water, mix the two solutions, stir vigorously at 60°C for 0.5 hour, and add NaOH to control the pH value of the mixture to 10.5. The obtained colloid is filtered or centrifugally dehydrated, washed with water until neutral, dried at 100°C, and placed at 500°C under N 2 Calcined in the atmosphere for 2 hours, the obtained sample was placed in a 10% glycerin aqueous solution by mass percentage, the pH value was controlled at 10.5, stirred at 60°C for 24 hours, the obtained colloid was filtered or centrifugally dehydrated, and dried at 100°C to obtain the desired catalyst. Take 5 L of glycerin aqueous solution with a concentration of 10% by mass, add the prepared catalyst with 10% by mass of glycerin, after heating up to 60°C, start to drop hydrogen peroxide with a concentration of 3.0% by mass, and rea...

Embodiment 2

[0026] 4.04 kg Fe(NO 3 ) 2 9H 2 O, 2.91 kg Co(NO 3 ) 2 ·6H 2 O and 3.75kg Al(NO 3 ) 3 9H 2 O was made into 20 L solution with deionized water; 1.06 kg Na 2 CO 3 Prepare 20 L solution with deionized water, mix the two solutions, stir vigorously at 60°C for 0.5 hour, and add NaOH to control the pH value of the mixture to 9.0. The obtained colloid is filtered or centrifugally dehydrated, washed with water until neutral, dried at 100°C, and placed at 300°C under N 2 Calcined in the atmosphere for 2 hours, the obtained sample was placed in an aqueous glycerin solution with a mass percent concentration of 10%, the pH value was controlled at 9.0, stirred at 60°C for 24 hours, the obtained colloid was filtered or centrifugally dehydrated, and dried at 100°C to obtain the desired catalyst. Take 5 L of glycerin aqueous solution with a mass percentage concentration of 10%, add the prepared catalyst with a mass percentage concentration of 10% glycerin, after heating up to 70°C, ...

Embodiment 3

[0028] 4.00 kg Cr(NO 3 ) 2 9H 2 O, 2.42 kg Cu(NO 3 ) 2 ·3H 2 O, 2.83 kg Mn(NO 3 ) 2 ·6H 2 O, 5.82 kg Ni(NO 3 ) 2 ·6H 2 O and 3.75 kg Al(NO 3 ) 3 9H 2 O was made into a 300 L solution with deionized water; 1.06 kg Na 2 CO 3 Prepare 300 L solution with deionized water, mix the two solutions, stir vigorously at 60°C for 0.5 hour, and add NaOH to control the pH value of the mixture to 10.0. The obtained colloid is filtered or centrifugally dehydrated, washed with water until neutral, dried at 100°C, and placed at 700°C under N 2 Calcined in the atmosphere for 2 hours, the obtained sample was placed in an aqueous glycerin solution with a mass percent concentration of 50%, the pH value was controlled at 10.0, stirred at 60°C for 24 hours, the obtained colloid was filtered or centrifugally dehydrated, and dried at 100°C to obtain the desired catalyst. Take 5 L of glycerin aqueous solution with a mass percentage concentration of 10%, add the prepared catalyst with a ma...

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Abstract

The invention discloses a method for preparing dihydroxy acetone by selectively oxidizing glycerin with hydrogen peroxide and belongs to the field of preparation of the dihydroxy acetone. The method comprises the following steps of: adding a transition metal hydrotalcite-like compound as a catalyst in 10 to 100 mass percent of glycerin aqueous solution, and controlling the dosage of the catalyst to be 5 to 20 percent of the mass of the glycerin; raising the temperature of a mixture to 25 to 90 DEG C by heating, dripping 3 to 50 mass percent of hydrogen peroxide, and reacting for 1 to 24 h; after reaction, centrifugally separating the catalyst from a reaction solution; and recovering the catalyst for reusing, and feeding the reaction solution to a liquid chromatogram for identification analysis. By using the glycerin and the hydrogen peroxide as raw materials, under the action of the transition metal hydrotalcite-like compound which serves as the catalyst, the conversion rate of the glycerin and the yield of the dihydroxy acetone are high; any acid base and any organic additive are not added in a reaction system; and the method has the advantages of high yield, low cost, no environmental pollution, easiness in separation, good repeatability, and the like.

Description

technical field [0001] The invention relates to a method for preparing dihydroxyacetone, in particular to a method for preparing dihydroxyacetone by selectively oxidizing glycerin with hydrogen peroxide. Background technique [0002] The increasingly scarce petroleum resources and the deteriorating environment force people to actively seek renewable clean energy to replace fossil energy, so the preparation of biodiesel from natural oils and fats has attracted much attention in recent years. In this process, for every ton of biodiesel produced, 100 kg of by-product glycerol will be produced. Therefore, in recent years, the production of glycerol has been increasing with the development of biodiesel industry, so it is urgent to find a new outlet for glycerin. Among the many uses of glycerol, the oxidation of glycerol to produce high value-added glyceric acid, glyceraldehyde, dihydroxyacetone, glycolic acid, etc. has a promising market prospect. [0003] Among them, dihydroxya...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/17C07C45/29B01J23/34B01J23/75B01J23/889
Inventor 吴功德王晓丽丁克强张方刘献锋孙雯宋晓波
Owner NANJING INST OF TECH
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