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A kind of method of catalytic oxidation synthesis glyceraldehyde acetone

A technology of glycerol aldehyde acetonide and glyceryl alcohol acetonide, which is applied in chemical instruments and methods, preparation of organic compounds, carbon-based compounds, etc., can solve the problems of needing membrane separation, not suitable for industrial production, and high energy consumption. Achieve the effects of mild conditions, easy industrialized large-scale production, and simple reaction operation

Active Publication Date: 2020-03-31
YANGZHOU POLYTECHNIC INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] There are also reports in the literature that glycerol is used as a raw material to synthesize glyceraldehyde by indirect electrooxidation. Although this method has the characteristics of simple reaction steps and high product yield, the energy consumption in the reaction is large, and membrane separation is required, so it is not suitable for industrial production.

Method used

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  • A kind of method of catalytic oxidation synthesis glyceraldehyde acetone
  • A kind of method of catalytic oxidation synthesis glyceraldehyde acetone
  • A kind of method of catalytic oxidation synthesis glyceraldehyde acetone

Examples

Experimental program
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Embodiment 1

[0040] (1) Take C 60 Mix fullerene (1.0g), 1mol / L zinc nitrate solution (2mL) and 1mol / L ammonia water (2.4mL) in an autoclave evenly, heat up to 120-125°C for 20h, then cool down to room temperature naturally Afterwards, after filtering, the precipitate was washed with deionized water and ethanol, and dried in vacuum at 80° C. for 6 h to obtain fullerene zinc oxide (C 60 / ZnO) material (hereinafter referred to as product a);

[0041] (2) Take product a (1.0 g) and add it into 10% ethanol solution (120 mL) by volume fraction and stir for 10-15 min, then add selenium-containing hydrazine hydrate (15 mL, containing 150 mg selenium), and continue stirring for 10-15 min, Raise the temperature to 175-180°C for 12 hours, then cool naturally to room temperature, filter, wash the precipitate with deionized water and ethanol, and vacuum dry at 70°C for 10 hours to obtain the fullerene zinc selenium oxide (C 60 / ZnO / Se) composite material (hereinafter referred to as product A).

Embodiment 2

[0043] (1) Take C 70 Fullerene (1.0g), 2mol / L zinc sulfate solution (1.5mL), and 1mol / L ammonia water (4.5mL) were mixed uniformly in an autoclave, and the temperature was raised to 125-130°C for 18 hours, and then naturally dropped to After room temperature, filter and precipitate, wash with deionized water and ethanol, and vacuum-dry at 60°C for 10 h to obtain fullerene zinc oxide (C 70 / ZnO) material (hereinafter referred to as product b);

[0044] (2) Take product b (1.0g) and add it into ethanol solution (180mL) with a volume fraction of 5% and stir for 10-15min, then add selenium-containing hydrazine hydrate (10mL, containing 60mg selenium), and continue stirring for 10-15min, After heating up to 160-165°C for 16 hours, cool naturally to room temperature, filter, wash the precipitate with deionized water and ethanol, and vacuum dry at 80°C for 6 hours to obtain the fullerene zinc selenium oxide (C 70 / ZnO / Se) composite material (hereinafter referred to as product B). ...

Embodiment 3

[0046] (1) After mixing graphene (1.0g), 1mol / L zinc nitrate solution (2mL), and 1mol / L ammonia water (2.4mL) in an autoclave, heat up to 120-125°C for 20 hours, and then naturally After cooling down to room temperature, filter and precipitate, wash with deionized water and ethanol, and vacuum-dry at 80°C for 6 hours to obtain a graphene zinc oxide material (hereinafter referred to as product c);

[0047] (2) Take product c (1.0g) and add it into 10% ethanol solution (120mL) by volume fraction and stir for 10-15min, then add selenium-containing hydrazine hydrate (15mL, containing 150mg selenium), and continue stirring for 10-15min, After heating up to 175-180°C for 12 hours, cool naturally to room temperature, filter and precipitate, wash with deionized water and ethanol, and vacuum-dry at 70°C for 10 hours to obtain a graphene zinc oxide selenium composite material (hereinafter referred to as product C).

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Abstract

The invention relates to a method for catalytic synthesis for glyceraldehyde acetonide. The method specifically comprises the following steps: dissolving glycerol acetonide into acetone, adding a proper amount of a fullerene zinc oxide selenium (C60 / ZnO / Se) composite material, introducing oxygen to carry out a reaction at a room temperature till a reaction liquid has no glycerol acetonide, centrifuging to remove the fullerene zinc oxide selenium (C60 / ZnO / Se) composite material, carrying out vacuum concentration on supernate, and drying to obtain the glyceraldehyde acetonide.

Description

technical field [0001] The invention belongs to the field of organic synthesis and catalysis, and in particular relates to a method for synthesizing glycerol aldehyde acetal by catalytic oxidation. Background technique [0002] Glyceraldehyde is the earliest discovered optically active aldose compound, which contains a pair of chiral carbon atoms, that is, D-type and L-type optical isomers, and is often used as a standard for calibrating carbohydrate configurations. Racemate D, L-glyceraldehyde has anti-glycolysis effect and is a good blood sugar protective agent. At the same time, as an important organic synthesis intermediate, it occupies an important role in the synthesis of medicine, agricultural chemicals and natural products. Quite an important position, it can be used as a chiral source in organic synthesis for asymmetric synthesis, especially it contains active functional groups-aldehyde groups, which can produce various types of derivatives, so it is very important ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/26B01J27/057C07C45/38C07C47/19
CPCB01J27/0573C07C45/38C07D317/26C07C47/19
Inventor 陈柯全刘伟罗志臣左志芳
Owner YANGZHOU POLYTECHNIC INST