Method for preparing 1,3-dihydroxyacetone catalyst from glycerinum

A hydroxyacetone catalyst and catalyst technology, which are applied in the preparation of organic compounds, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve the problems of Au sintering and particle size, insufficient activity, and low utilization rate of active components. , to achieve the effect of increasing surface area and stability, good activity and selectivity, and enriching loaded active sites

Active Publication Date: 2019-03-22
JIANGXI NORMAL UNIV
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  • 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 effect of surface tension leads to Au sintering and particle enlargement, which is easy to be lost 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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  • Method for preparing 1,3-dihydroxyacetone catalyst from glycerinum

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Embodiment 1

[0021] A preparation method for preparing 1,3-dihydroxyacetone catalyst, comprising the steps of:

[0022] (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 solution B, then quickly mix solution A and solution B under rapid stirring, and reflux reaction at 60°C for 10h. After the reaction, the product is centrifugally washed to neutral, Dry to get ZnAl-HTLc;

[0023] (2) Preparation of composite carrier: Add 80mL of ZnAl-HTLc12g prepared in step (1) into 0.6mol / L glucose monohydrate aqueous solution, stir at room temperature until uniformly mixed; then transfer the above mixture to poly In a tetrafluoroethylene reactor, react at a constant temperature of 180°C for 6 hours, cool to room temperature after the reaction, separate the product, then alternately wash with deionized wat...

Embodiment 2

[0026] A preparation method for preparing 1,3-dihydroxyacetone catalyst, comprising the steps of:

[0027] (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 3Dissolve 0.32g NaOH in 150ml deionized water to prepare mixed solution B, then quickly mix solution A and solution B under rapid stirring, and reflux reaction at 60°C for 10h. After the reaction, the product is centrifugally washed to neutral, Dry to get ZnAl-HTLc;

[0028] (2) Preparation of composite carrier: Add 15g of ZnAl-HTLc prepared in step (1) into 80mL of glucose monohydrate aqueous solution with a concentration of 0.6mol / L, stir at room temperature until uniformly mixed; then transfer the above mixture to poly In a tetrafluoroethylene reactor, react at a constant temperature of 180°C for 6 hours, cool to room temperature after the reaction, separate the product, then alternat...

Embodiment 3

[0031] A preparation method for preparing 1,3-dihydroxyacetone catalyst, comprising the steps of:

[0032] (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 solution B, then quickly mix solution A and solution B under rapid stirring, and reflux reaction at 60°C for 10h. After the reaction, the product is centrifugally washed to neutral, Dry to get ZnAl-HTLc;

[0033] (2) Preparation of the composite carrier: add the ZnAl-HTLc12g prepared in step (1) into 100mL, and the concentration is 0.5mol / L in the aqueous glucose monohydrate solution, and stir at room temperature until uniformly mixed; then transfer the above mixture to poly In a tetrafluoroethylene reactor, react at a constant temperature of 180°C for 6 hours, cool to room temperature after the reaction, separate the product...

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Abstract

The invention discloses a method for preparing a 1,3-dihydroxyacetone catalyst from glycerinum. The method comprises the following steps: (1) preparing ZnAl-HTLc, namely dissolving a zinc salt and analuminum salt into deionized water so as to obtain a solution A, preparing a solution B from Na2O3 and NaOH, rapidly mixing the solution A with the solution B, carrying out a backflow reaction, carrying out centrifugal washing and drying after the reaction so as to obtain ZnAl-HTLc; (2) preparing a composite carrier, namely uniformly mixing the prepared ZnAl-HTLc into a glucose monohydrate solution, transferring the mixture into a polytetrafluoroethylene reaction kettle, carrying out a hydrothermal reaction, cooling, washing, and drying so as to obtain a ZnAl-HTLc/carbon composite carrier; and(3) preparing a catalyst, namely preparing solutions from cupric nitrate, lanthanum nitrate and cobalt nitrate respectively, putting the solutions into the composite carrier simultaneously, soaking,drying, roasting, and carrying out hydrogen activation, thereby obtaining the catalyst. The catalyst prepared by using the method is high in activity, selectivity and stability, and is wide in application prospect.

Description

technical field [0001] The invention belongs to the field of catalysts, in particular to a preparation method for preparing 1,3-dihydroxyacetone catalyst from glycerin. 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 prepared by microbia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83C07C45/39C07C49/17
CPCB01J23/83C07C45/39C07C49/17
Inventor 王宝荣廖维林郭韬芮培欣谢贤清
Owner JIANGXI NORMAL UNIV
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