Preparation technique of 1,3-dihydroxyacetone

A technology for the preparation of dihydroxyacetone, which is applied in the field of preparation of 1,3-dihydroxyacetone, can solve the problems of Au sintering and particle enlargement, insufficient activity, and low utilization rate of active components, etc., to increase the surface area and Stability, enhanced activity and selectivity, and the effect of enriching active sites

Inactive Publication Date: 2019-03-22
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the specific surface area of ​​ZnO is generally low, which is not conducive to the dispersion of Au when used as a carrier.
Especially at high loads, the surface tension causes Au to sinter and the particles become larger, which is easy to lose and the utilization rate of precious metals is low
[0004] However, the above-mentioned catalysts generally have the defects of low utilization rate of active components, insufficient activity, and insufficient stability, dispersion and specific surface area of ​​the carrier components, resulting in insufficient selectivity of 1,3-dihydroxyacetone. To develop a Catalysts with excellent activity are necessary

Method used

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  • Preparation technique of 1,3-dihydroxyacetone

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Embodiment 1

[0023] A preparation process of 1,3-dihydroxyacetone, the specific steps are as follows: add glycerin aqueous solution and catalyst into the high-pressure reaction kettle, after the airtightness is complete, use high-purity oxygen to evacuate three times at room temperature, and then fill it with 1.0MPa high-pressure reactor. Pure oxygen, stirred and heated to 80°C, reacted at constant temperature for 3 hours, cooled to room temperature with ice bath, centrifuged and filtered, and the reaction liquid was detected by high performance liquid chromatography to measure the conversion rate of glycerol and the selectivity of 1,3-dihydroxyacetone;

[0024] The preparation method of catalyst described in the present embodiment is:

[0025] (1) Preparation of ZnAl-HTLc: soluble 0.375gAl(NO 3 ) 3 9H 2 O, 0.891gZn(NO 3 ) 2 ·6H 2 O was dissolved in 150ml of deionized water to prepare mixed solution A, and 0.042gNa 2 CO 3 Dissolve 0.48g NaOH in 150ml deionized water to prepare mixed...

Embodiment 2

[0029] A preparation process of 1,3-dihydroxyacetone, the specific steps are as follows: add glycerin aqueous solution and catalyst into the high-pressure reaction kettle, after the airtightness is complete, use high-purity oxygen to evacuate three times at room temperature, and then fill it with 1.0MPa high-pressure reactor. Pure oxygen, stirred and heated to 80°C, reacted at constant temperature for 3 hours, cooled to room temperature with ice bath, centrifuged and filtered, and the reaction liquid was detected by high performance liquid chromatography to measure the conversion rate of glycerol and the selectivity of 1,3-dihydroxyacetone;

[0030] The preparation method of catalyst described in the present embodiment is:

[0031] (1) Preparation of ZnAl-HTLc: soluble 0.375gAl(NO 3 ) 3 9H 2 O, 0.594gZn(NO 3 ) 2 ·6H 2 O was dissolved in 150ml of deionized water to prepare mixed solution A, and 0.042gNa 2 CO 3 Dissolve 0.32g NaOH in 150ml deionized water to prepare mixed s...

Embodiment 3

[0035] A preparation process of 1,3-dihydroxyacetone, the specific steps are as follows: add glycerin aqueous solution and catalyst into the high-pressure reaction kettle, after the airtightness is complete, use high-purity oxygen to evacuate three times at room temperature, and then fill it with 1.0MPa high-pressure reactor. Pure oxygen, stirred and heated to 80°C, reacted at constant temperature for 3 hours, cooled to room temperature with ice bath, centrifuged and filtered, and the reaction liquid was detected by high performance liquid chromatography to measure the conversion rate of glycerol and the selectivity of 1,3-dihydroxyacetone;

[0036] The preparation method of catalyst described in the present embodiment is:

[0037] (1) Preparation of ZnAl-HTLc: soluble 0.375gAl(NO 3 ) 3 9H 2 O, 0.891gZn(NO 3 ) 2 ·6H 2 O was dissolved in 150ml of deionized water to prepare mixed solution A, and 0.05gNa 2 CO 3 Dissolve 0.40g NaOH in 150ml deionized water to prepare mixed ...

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Abstract

The invention discloses a preparation technique of 1,3-dihydroxyacetone. The technique specifically comprises the steps as follows: adding a glycerin aqueous solution and a catalyst into a high-pressure reaction kettle, sealing the reaction kettle completely, evacuating air three times with high-purity oxygen at room temperature, then filling the reaction kettle with 1.0MPa high-purity oxygen, stirring and heating to 70-90 DEG C, reacting at a constant temperature for 2-5h, cooling to room temperature with an ice bath, centrifuging, filtering and separating a reaction solution to obtain 1,3-dihydroxyacetone, wherein the catalyst comprises a carrier and active components, the carrier is a ZnAl-HTLc / carbon composite carrier, and the active components comprise Au, Bi and Ce. The catalyst prepared in the invention has very good glycerin conversion rate and selectivity on 1,3-dihydroxyacetone, thereby having broad application prospects.

Description

technical field [0001] The invention belongs to the technical field of preparation of 1,3-dihydroxyacetone, and in particular relates to a process for preparing 1,3-dihydroxyacetone. Background technique [0002] 1,3-Dihydroxyacetone (DHA for short) is the simplest ketose sugar, which is easily soluble in organic solvents such as water, ethanol, acetone and ether. DHA is an important chemical raw material, widely used in fine chemical industry, food, cosmetics and water purification and other industries; at the same time, DHA is also an important organic synthesis intermediate, which can be used to prepare various chiral compounds by aldol condensation and reduction preparation Optically active secondary alcohols, Diels-Alder addition to prepare sugar compounds or further reactions for such addition reactions, insertion reactions with carbene, and preparations with 2,2-dialkoxycyclopropane derivatives Lactone, etc. [0003] At present, 1,3-dihydroxyacetone is mainly prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/39B01J23/68C07C49/17
CPCB01J23/681C07C45/39C07C49/17
Inventor 王宝荣芮培欣谢贤清郭韬廖维林
Owner JIANGXI NORMAL UNIV
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