Oxygen vacancy-rich ferric oxide nitrogen fixation catalyst based on reducing ionic liquid, preparation method and its electrocatalytic nitrogen fixation application

A ferric oxide, ionic liquid technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., can solve the complex preparation operation, ammonia yield and Faradaic efficiency Can not meet the requirements of industrial production, complex preparation methods and other problems, to achieve the effects of cheap and easily available raw materials, excellent nitrogen reduction catalytic performance, and simple preparation methods

Inactive Publication Date: 2020-05-01
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, it is also reported that iron group catalysts are mixed with other substances, such as ferric oxide mixed with carbon nanotubes, and through the synergistic effect of ferric oxide and carbon nanotubes, higher ammonia production can be obtained at normal temperature and pressure. and Faraday efficiency; however, its preparation process requires a variety of raw materials, and the preparation method is relatively complicated
At the same time, the ammonia production and Faradaic efficiency of the above two methods cannot meet the requirements of industrial production
[0004] In order to further improve the catalytic performance of the catalyst, defect design is also an important means; at present, ferric oxide rich in oxygen vacancies has been widely used in catalytic reactions; however, the preparation of ferric oxide rich in oxygen vacancies often requires two steps. Reaction, that is, to prepare ferric oxide first, and then burn the obtained ferric oxide at high temperature or etch with inert gas, the preparation operation is more complicated

Method used

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  • Oxygen vacancy-rich ferric oxide nitrogen fixation catalyst based on reducing ionic liquid, preparation method and its electrocatalytic nitrogen fixation application
  • Oxygen vacancy-rich ferric oxide nitrogen fixation catalyst based on reducing ionic liquid, preparation method and its electrocatalytic nitrogen fixation application
  • Oxygen vacancy-rich ferric oxide nitrogen fixation catalyst based on reducing ionic liquid, preparation method and its electrocatalytic nitrogen fixation application

Examples

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Effect test

Embodiment 1

[0037]A method for preparing an oxygen-vacancy-rich ferric oxide nitrogen-fixing catalyst based on reducing ionic liquids, comprising the steps of:

[0038] In an ice-water bath (0°C), add formic acid drop by drop to octylamine (the molar ratio of formic acid and octylamine is 1:1), stir while adding dropwise, after the dropwise addition, stir and mix evenly until no white smoke, a white solid was obtained, that is, a reducing ionic liquid (OAF) was successfully synthesized.

[0039] 30mg (1.1×10 -4 mol) FeCl 3 ·6H 2 O and 4g (0.023mol) of OAF were thoroughly mixed evenly, then placed in a closed reactor, and subjected to ionothermal reaction at 180°C for 12 hours; after the reaction was completed, cooled to room temperature, centrifuged, washed 4 times with absolute ethanol and deionized water, and then The product was put into a vacuum drying oven and dried at room temperature for 12 hours to obtain a brown-red solid powder, which is a nitrogen fixation catalyst rich in o...

Embodiment 2

[0052] A method for preparing an oxygen-vacancy-rich ferric oxide nitrogen-fixing catalyst based on reducing ionic liquids, comprising the steps of:

[0053] In an ice-water bath (0°C), add formic acid drop by drop to octylamine (the molar ratio of formic acid and octylamine is 1:1), stir while adding dropwise, after the dropwise addition, stir and mix evenly until no white smoke, a white solid was obtained, that is, a reducing ionic liquid (OAF) was successfully synthesized.

[0054] 30mg (1.1×10 -4 mol) FeCl 3 ·6H 2 O and 2g (0.012mol) of OAF were thoroughly mixed evenly, then placed in a closed reactor, and subjected to ionothermal reaction at 140°C for 15 hours; after the reaction was completed, cooled to room temperature, centrifuged, washed 4 times with absolute ethanol and deionized water, and then The product was put into a vacuum oven and dried at room temperature for 10 h to obtain a brown-red solid powder.

Embodiment 3

[0056] A method for preparing an oxygen-vacancy-rich ferric oxide nitrogen-fixing catalyst based on reducing ionic liquids, comprising the steps of:

[0057] In an ice-water bath (0°C), add formic acid drop by drop to octylamine (the molar ratio of formic acid and octylamine is 1:1), stir while adding dropwise, after the dropwise addition, stir and mix evenly until no white smoke, a white solid was obtained, that is, a reducing ionic liquid (OAF) was successfully synthesized.

[0058] 30mg (1.1×10 -4 mol) FeCl 3 ·6H 2 O and 6g (0.035mol) of OAF were thoroughly mixed evenly, then placed in a closed reactor, and subjected to ionothermal reaction at 220°C for 8 hours; after the reaction was completed, cooled to room temperature, centrifuged, washed 4 times with absolute ethanol and deionized water, and then The product was put into a vacuum oven and dried at room temperature for 15 hours to obtain a brown-red solid powder.

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Abstract

The invention provides a reductive ionic liquid-based iron trioxide nitrogen-fixation catalyst rich in oxygen vacancy, a preparation method and electro-catalysis nitrogen-fixation application of the iron trioxide nitrogen-fixation catalyst. The preparation method of the catalyst comprises the steps that formic acid and octylame are mixed under stirring to obtain reductive ionic liquid; an iron source and the reductive ionic liquid are fully mixed, and the iron trioxide nitrogen-fixation catalyst is obtained through an ionothermal reaction, centrifugation, washing and drying. The raw materialsare low in prices and easy to obtain, the operation is simple, the cost is low, and large-scale application is facilitated. The prepared iron trioxide nitrogen-fixation catalyst is nanometer cubic iron trioxide particles which are rich in oxygen vacancy and small in particle size, and when used for electro-catalysis nitrogen fixation, the catalyst has excellent nitrogen reduction and catalysis performance.

Description

technical field [0001] The invention relates to a ferric oxide nitrogen fixation catalyst rich in oxygen vacancies based on a reducing ionic liquid, a preparation method and an electrocatalytic nitrogen fixation application thereof, belonging to the technical field of energy materials. Background technique [0002] Convert atmospheric nitrogen to NH 3 It is a major achievement in the history of human society, and the obtained NH 3 It can be further processed into fertilizer, etc., to provide more resources for the continuously growing world population. Traditional industrial production of NH 3 The most common method is the Haber-Bosch method, which is to combine nitrogen and hydrogen into ammonia under high temperature and pressure; this method requires high energy consumption, and a large amount of greenhouse gas CO will be produced in the process of hydrogen production. 2 . Therefore, people pay more and more attention to the green and low-cost synthesis technology of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745B01J35/02B01J37/00B01J37/08B01J37/16C25B1/00C25B11/06B82Y40/00
CPCB01J23/745B01J35/0013B01J35/0033B01J35/023B01J35/026B01J37/0018B01J37/08B01J37/16B82Y40/00C25B1/00C25B11/077
Inventor 李钟号张晨韵
Owner SHANDONG UNIV
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