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Method for preparing polycarboxylic acid by electrocatalytic oxidation of aldehydes and alcohols

An electrocatalytic oxidation, polycarboxylic acid technology, applied in electrodes, electrolysis components, electrolysis process and other directions, can solve the problems of large oxidant, low selectivity of glucaric acid, high cost, etc., and achieve low preparation cost, excellent stability, The effect of multiple active sites

Pending Publication Date: 2022-06-03
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional catalytic oxidation of glucose to glucaric acid has several disadvantages: (1) a large amount of toxic oxidizing agent is required (more than twice the stoichiometric ratio); (2) the selectivity to glucaric acid is low (the selection of glucaric acid (3) produces various chemically similar by-products (such as tartaric acid, glycolic acid, hydroxymalonic acid and oxalic acid); (4) uses high-pressure oxygen, which hides safety risks; (5) precious metals (such as Scarcity of Pt, Ru, Rh, and Pd)-based catalysts brings high cost

Method used

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  • Method for preparing polycarboxylic acid by electrocatalytic oxidation of aldehydes and alcohols
  • Method for preparing polycarboxylic acid by electrocatalytic oxidation of aldehydes and alcohols
  • Method for preparing polycarboxylic acid by electrocatalytic oxidation of aldehydes and alcohols

Examples

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Effect test

Embodiment 1

[0033] Example 1 A method for constructing an electrocatalytic system that couples Fe LDH nanosheets of polyacids prepared by oxidation of biomass and nitroxide free radical compounds.

[0034] Pretreatment of carbon felt: Sonicate commercial carbon felt in absolute ethanol and distilled water for 4 minutes, wash to remove surface impurities, then use carbon felt as working electrode, platinum sheet as counter electrode, mercury / mercury oxide electrode as reference electrode, 1M NaOH solution is the electrolyte, and it is oxidized by chronopotentiometry. After the treatment, the carbon felt is ultrasonically washed with a large amount of distilled water for 30 minutes to remove residual NaOH. In the chronopotentiometry, the potential is 1.9V (vs. RHE), and the processing time is 10min.

[0035]Dissolve 0.2 g of urea and 0.1 g of ferric nitrate in deionized water, add absolute ethanol, stir, and ultrasonically mix for 10 min to obtain a yellow clear solution. Transfer the solu...

Embodiment 2

[0039] Example 2 A method for constructing an electrocatalytic system coupled with Ni LDH nanosheets and nitroxide radical compounds for the preparation of polybasic acids by oxidation of biomass

[0040] Dissolve 1 g of urea and 1 g of nickel nitrate in deionized water, add absolute ethanol, stir, and ultrasonically mix for 10 minutes to obtain a green clear solution. Transfer the solution to the PTFE lining, put a piece of carbon felt, seal it in a hydrothermal autoclave, and keep it warm at 160°C for 16h. After cooling down, wash with ethanol and distilled water for several times in sequence to obtain the precursor. After drying the precursor in an oven at 60°C for 1 hour, the precursor is calcined in a muffle furnace, and the temperature is programmed at a rate of 5°C / min in an air atmosphere to 400°C and keep it for 4h to get the final NiO-CF catalyst. Before the catalyst is officially used, it needs to be activated in the reaction system.

[0041] The NiO-CF prepared a...

Embodiment 3

[0043] Example 3 A method for constructing an electrocatalytic system coupled with Co LDH nanosheets and nitroxide free radical compounds for the preparation of polybasic acids by oxidation of biomass

[0044] Dissolve 1.5 g of urea and 1 g of cobalt nitrate in deionized water, add absolute ethanol, stir, and ultrasonically mix for 10 minutes to obtain a red clear solution. Transfer the solution to the PTFE lining, put a piece of carbon felt, seal it in a hydrothermal autoclave, and keep it warm at 170°C for 20h. After cooling down, wash with ethanol and distilled water for several times in sequence to obtain the precursor. After drying the precursor in an oven at 60°C for 1 hour, the precursor is calcined in a muffle furnace, and the temperature is programmed at a rate of 5°C / min in an air atmosphere to 450°C and keep for 4h to get the final Co 3 o 4 - CF catalyst. Before the catalyst is officially used, it needs to be activated in the reaction system.

[0045] The above ...

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Abstract

A method for preparing polycarboxylic acid by electrocatalytic oxidation of aldehydes and alcohols belongs to the technical field of electrocatalytic materials, and comprises the following steps: taking a carbon felt loaded with transition metal as an anode, taking a platinum sheet electrode as a cathode, and separating two electrodes of an electrolytic tank by an anionic membrane to form an electrocatalytic reactor; the polybasic carboxylic acid is prepared by performing electrocatalytic oxidation on an aldehyde alcohol substance through direct current low voltage in an electrolyte containing a nitroxide free radical compound or a derivative thereof, the aldehyde alcohol substance and an inorganic salt. Taking glucose as an example, compared with an existing strong-alkali electrocatalysis system, the system can effectively reduce side reactions such as anti-aldol and the like under the weak-alkali mild condition, the glucaric acid selectivity is remarkably improved, meanwhile, hydrogen is co-produced, and the system has universality in the aspect of aldol biomass molecular oxidation.

Description

technical field [0001] The invention relates to the field of organic electrochemical catalysis, in particular to a method for preparing polycarboxylic acids by electrocatalytically oxidizing aldols. Background technique [0002] Biomass resources with high oxygen content are ideal raw materials for the production of oxygenated chemicals. Among them, cellulose plays a very important role in the field of catalytic conversion of biomass. Based on the hydrolysis of cellulose to prepare glucose, oxidizing glucose to prepare glucaric acid through glucaric acid, and then hydrogenolyzing glucaric acid to prepare adipic acid, an important chemical raw material, is a very economical transformation path. Furthermore, 5-hydroxymethylfurfural (HMF) is a platform chemical prepared by acid-catalyzed dehydration of glucose or fructose or hydrolysis-dehydration of polysaccharides. Hydroxyl or aldehyde groups on HMF are oxidized to produce valuable chemicals, especially 2,5-furandicarboxyli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/23C25B3/07C25B3/05C25B11/065C25B11/095C25B1/04C23C18/12
CPCC25B3/23C25B3/07C25B3/05C25B11/065C25B11/095C25B1/04C23C18/1216C23C18/1245
Inventor 邓卫平张凯王瑶张庆红王野
Owner XIAMEN UNIV
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