Ruthenium-based ammonia synthesis catalyst with nitrogen-doped activated carbon as carrier and preparation method thereof

A technology of activated carbon and nitrogen doping, which is used in the preparation/separation of ammonia, chemical instruments and methods, catalysts for physical/chemical processes, etc. Change electron density and structure, improve activity and stability, and enhance the effect of alkalinity

Active Publication Date: 2019-06-11
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In recent years, with the development of carbon materials, many new composite carbon materials have been derived, and the research on the modification and modification of the surface of carbon materials is also advancing steadily. Among them, nitrogen-doped carbon materials have emerged in the fields of electrochemistry and sensors. The patent No. CN104785255A reports a ruthenium-based ammonia synthesis catalyst using urea as a nitrogen source. The specific surface area of ​​its preparation is low, and its activity is not as high as that of the present invention; secondly, the nitrogen prepared by this method has an indeterminate form , uncontrollable functional groups and other disadvantages

Method used

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preparation example Construction

[0025] A preparation method of a ruthenium-based ammonia synthesis catalyst taking nitrogen-doped activated carbon as a carrier, comprising the following steps:

[0026] (1) Pretreatment of activated carbon: graphitize the activated carbon in an inert atmosphere and at a temperature of 2050-2150°C, and then carry out pore expansion, crushing, sieving, washing and drying on the graphitized activated carbon in sequence ;

[0027] (2) Preparation of nitrogen-doped activated carbon: Mix the above-mentioned activated carbon and melamine at a mass ratio of 1:1 to 5, and then mix the mixture of activated carbon and melamine with anhydrous Mix ethanol with magnetic stirring, and heat and reflux in a constant temperature water bath for 3 to 20 hours. After the treatment, the mixture is placed in a drying oven at 95 to 105°C for 11 to 13 hours. Put it into the tube furnace, and pass through the protective gas. Under the inert atmosphere of the protective gas, raise the temperature of t...

Embodiment 1

[0039] A preparation method of a ruthenium-based ammonia synthesis catalyst taking nitrogen-doped activated carbon as a carrier, comprising the following steps:

[0040](1) Pretreatment of activated carbon: take 10g of activated carbon and carry out graphitization treatment at a temperature of 2100°C in an inert atmosphere, then perform hole expansion treatment on the activated carbon, and crush the activated carbon after the hole expansion, and pass through a 14-mesh screen Sieved before washing and drying;

[0041] (2) Preparation of nitrogen-doped activated carbon: Mix 4 g of the above-mentioned activated carbon and 10 g of melamine, then magnetically stir the mixture of activated carbon and melamine with absolute ethanol at a liquid-solid ratio of 18 ml / g, and mix at 60 ℃ constant temperature water bath to heat and reflux for 10h. After the treatment, the mixture was dried in a drying oven at 100℃ for 12h. Introduce nitrogen, under the nitrogen atmosphere, raise the tempe...

Embodiment 2

[0047] A preparation method of a ruthenium-based ammonia synthesis catalyst taking nitrogen-doped activated carbon as a carrier, comprising the following steps:

[0048] (1) Pretreatment of activated carbon: take 10g of activated carbon and carry out graphitization treatment under the condition of inert atmosphere and temperature of 2100°C, then carry out pore expansion treatment on activated carbon, and crush the activated carbon after pore expansion, and pass through a 14-mesh sieve Mesh sieving before washing and drying;

[0049] (2) Preparation of nitrogen-doped activated carbon: Mix 4 g of the above-mentioned activated carbon and 10 g of melamine, then magnetically stir the mixture of activated carbon and melamine with absolute ethanol at a liquid-solid ratio of 18 ml / g, and mix at 65 ℃ constant temperature water bath to heat and reflux for 10h. After the treatment, the mixture was dried in a drying oven at 100℃ for 12h. Introduce nitrogen, and under nitrogen atmosphere,...

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Abstract

The invention discloses a ruthenium-based ammonia synthesis catalyst adopting nitrogen doped activated carbon as a carrier and a preparation method thereof. A precursor of a nitrogen source of nitrogen doped activated carbon is melamine, the nitrogen doping amount is 0.72% to 7.61%, and the nitrogen source comprises the following main components by content: 1% to 15% of graphite nitrogen, 25% to 35% of pyridine nitrogen and 55% to 70% of pyrrole nitrogen. The preparation method comprises the steps of pretreatment of activated carbon, preparation of nitrogen doped activated carbon, preparation of an impregnation precursor solution, and preparation of the catalyst. According to the catalyst prepared through the method, the activity is high, the stability is good, the implementation is easy, and industrial popularization and utilization are facilitated.

Description

technical field [0001] The invention relates to the field of ammonia synthesis catalysts, in particular to a ruthenium-based ammonia synthesis catalyst with nitrogen-doped activated carbon as a carrier and a preparation method thereof. Background technique [0002] The ammonia synthesis industry has always been a pillar industry of the national economy, and the design and research of ammonia synthesis catalysts has always been a hot topic in catalytic chemistry research. In November 1992, the graphitized activated carbon-supported ruthenium-based ammonia synthesis catalyst and its process (KAAP) were jointly developed by BP Company of the United Kingdom and Kellogg Company of the United States, and industrialized for the first time in the Ocelot ammonia synthesis plant in Canada. Compared with traditional iron-based catalysts, ruthenium is more active. In the wave of building an environment-friendly and resource-saving society, ruthenium-based ammonia synthesis catalysts ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24C01C1/04
CPCY02P20/52
Inventor 林建新徐家祺倪军林炳裕江莉龙
Owner FUZHOU UNIV
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