Ruthenium ammonia synthesis catalyst with high-specific-surface-area graphite as carrier and preparation of ruthenium ammonia synthesis catalyst

A high specific surface area, catalyst technology, applied in catalyst carrier, ammonia preparation/separation, chemical instruments and methods, etc., can solve the problems of low specific surface area and small pore volume of ordinary graphite, and achieve high catalyst activity and simple equipment structure. Effect

Active Publication Date: 2014-09-03
FUZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a ruthenium-based ammonia synthesis catalyst with high specific surface graphite as a carrier and its preparation method, which is used t

Method used

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  • Ruthenium ammonia synthesis catalyst with high-specific-surface-area graphite as carrier and preparation of ruthenium ammonia synthesis catalyst
  • Ruthenium ammonia synthesis catalyst with high-specific-surface-area graphite as carrier and preparation of ruthenium ammonia synthesis catalyst

Examples

Experimental program
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Example Embodiment

[0021] Example 1

[0022] (1) Weigh 4.00g graphite and 20.00g magnetic steel needle (magnet needle size 1mm) into a closed 400mL glass container filled with air; use a water bath to control the temperature to 40℃ , Continue to run for different t time at 1800 r / min speed, then add 20mL of deionized water and continue to rotate for 2h, then settle and filter to separate and dry to obtain high specific surface graphite solid powder; high specific surface graphite physical weaving prepared by different magnetic grinding time The structure is shown in Table 1 below;

[0023] Table 1 Physical texture of high specific surface graphite obtained under different magnetic grinding time

[0024]

[0025] (2) Preparation of potassium ruthenate: Put ruthenium powder and potassium hydroxide in a nickel crucible and mix them evenly, and treat them in a muffle furnace at 400°C for 4 hours to obtain potassium ruthenate;

[0026] (3) Preparation of catalyst: The high specific surface graphite carrier ...

Example Embodiment

[0028] Example 2

[0029] Change the graphite mass m and replace the magnetic grinding container with a 200mL glass container. The magnetic grinding time is 12h. Other conditions are the same. The physical texture of the large surface graphite prepared by the same procedure is shown in Table 2.

[0030] Table 2 Physical texture of large surface graphite prepared with different ball-to-material ratios

[0031]

[0032] (2) Preparation of potassium ruthenate: Put ruthenium powder and potassium hydroxide in a nickel crucible and mix them evenly, and treat them in a muffle furnace at 650°C for 1 hour to obtain potassium ruthenate. The content of ruthenium is 4% of the carrier mass;

[0033] (3) Preparation of the catalyst: the high specific surface graphite support HAG-5 obtained in step (1) was immersed in the potassium ruthenate solution obtained in step (2) by an equal volume impregnation method, and the temperature was controlled at 60℃ each time The immersion time is 3min; the immer...

Example Embodiment

[0035] Example 3

[0036] Take the ordinary graphite in Example 2 as the carrier, the content of ruthenium is 4% of the carrier mass, the amount of auxiliary Ba is 2% of the carrier mass, the ratio of hydrogen to nitrogen in the mixed gas is 3:1, and the space velocity is 10000 h -1 , The tableting pressure is 10 MPa and the reaction temperature is 400 ℃, the optimal activity of the ruthenium-based ammonia synthesis catalyst is 2.3%.

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Abstract

The invention discloses a ruthenium ammonia synthesis catalyst with high-specific-surface-area graphite as a carrier and a preparation of the ruthenium ammonia synthesis catalyst. The ruthenium ammonia synthesis catalyst comprises Ru-Ba/HAG, wherein Ru refers to an active ingredient ruthenium accounting for 1-8% of the mass of the carrier; Ba refers to assistant barium accounting for 1-10% of the mass of the carrier; HAG refers to the graphite with a high specific surface area. With the high-specific-surface-area graphite as the carrier, the ammonia synthesis catalyst is prepared by preparing potassium ruthenate, supporting the catalyst, pressing and forming. The high-specific-surface-area graphite has relatively large specific surface area and porous volume and can provide enough space for metal dispersion; the surface energy is singular to provide the precondition for obtaining uniform metallic particles; the activity of the catalyst taking the high-specific-surface-area graphite as the carrier is higher than that of the catalyst taking ordinary graphite as the carrier; the surface functional groups of the graphite can be adjusted through different atmospheres, so as to obtain high-specific-surface-area graphite with different kinds and different quantity of surface functional groups; the high-specific-surface-area graphite has different characteristics when being used as the carrier of the ruthenium ammonia synthesis catalyst.

Description

technical field [0001] The invention belongs to the technical field of ammonia synthesis catalyst preparation, and more specifically relates to a ruthenium-based ammonia synthesis catalyst with high specific surface graphite as a carrier and a preparation method thereof. Background technique [0002] In the field of ammonia synthesis catalysts, activated carbon or graphitized activated carbon as a carrier has the highest ruthenium-based ammonia synthesis activity, but in the presence of ruthenium, carbon can undergo a methanation reaction with hydrogen, one of the reactants for ammonia synthesis, resulting in the loss of the carrier. The catalyst structure collapses. The industrialization process of carbon-supported catalysts is restricted by the stability of carbon supports, so it is still difficult to widely promote carbon-supported ruthenium-based ammonia synthesis catalysts. In laboratory research, graphitized activated carbon has better stability and activity, so choos...

Claims

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Application Information

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IPC IPC(8): B01J23/58B01J35/10B01J32/00C01C1/04
CPCY02P20/52
Inventor 倪军魏可镁刘本耀
Owner FUZHOU UNIVERSITY
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