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Catalysis type ammonia prepn. method, and method of prepn. and recovery of catalyst of ammonia synthesis

A catalyst, catalytic activity technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical recovery, etc., can solve the problems of loss of carbon support, sensitivity to hydrogenation, difficult operation, etc.

Inactive Publication Date: 2004-10-13
HALDOR TOPSOE AS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A general disadvantage of ruthenium catalysts is the use of carbon supports under industrial conditions, since all forms of carbon are susceptible to hydrogenation under these conditions
Hydrogenation leads to a gradual loss of carbon support through the formation of methane and ultimately serious operational difficulties

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of ruthenium catalysts.

[0024] The MgO support was purchased from Johnson-Matthey (purity 99.9955%, surface area 51.3m 2 / g). By using Ru 3 (CO) 12 impregnating the support in THF, or by Ru 3 (CO) 12 The chemical vapor deposition (CVD) of ruthenium is introduced on the carrier. On the other hand, available such as RuCl 3 A suitable salt of ruthenium is impregnated in a non-aqueous solvent. After drying the impregnated catalyst to remove the solvent or directly using CVD method deposited Ru 3 (CO) 12 / MgO, the catalyst was activated by treatment with hydrogen. Activation is at 30000h -1 and a heating rate of 0.1°C / min until it reached 550°C, at which point the catalyst was kept for 12 hours and cooled to room temperature. The catalyst was slowly exposed to ambient conditions (passivation) to minimize oxidation of the small Ru crystals. Activation can also be carried out in nitrogen-hydrogen-ammonia mixtures. A suitable Ru concentration range is...

Embodiment 2

[0026] Catalyst boost.

[0027] From Example 1, by adding Ru 3 (CO) 12 Catalysts prepared by CVD on MgO, subsequently activated and passivated with hydrogen, are promoted by impregnation of suitable promoter salts in non-aqueous solutions. Suitable promoters are alkali metals, alkaline earth metals, lanthanides and combinations thereof. In impregnation with accelerator salts, carbonates, hydroxides and nitrates are among the suitable counterions. In the separation reduction method as described in Example 1, the counterions can be removed, or they can be introduced directly into the catalytic converter. The optimum content of the promoter depends on the Ru concentration and dispersion, but is in the range of 0.2-5.0 moles of promoter per mole of ruthenium.

Embodiment 3

[0029] Catalyst detection.

[0030] The promoted Ru / MgO catalyst was transferred to the apparatus for catalytic activity measurement. The catalyst is heated to the desired detection temperature, typically 400 °C, and the pressure is increased to the desired detection pressure, typically 100 bar (100 x 10 5 KPa). at the required space velocity, typically 30000h -1 , pass a known hydrogen-nitrogen mixture and optionally ammonia over the catalyst bed, and determine the concentration of ammonia at the outlet. By systematically changing the temperature, pressure, space velocity and ammonia inlet concentration, under the corresponding conditions, that is, at a temperature of 300-550°C and a pressure of 10-140bar (10-140×10 5 KPa), the space velocity is 10000-100000h -1 The catalyst properties were evaluated between and at inlet concentrations of ammonia ranging from 0-20% by volume.

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PUM

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Abstract

A catalyst active in ammonia synthesis with improved activity and a process for the recovery of useful components from the catalyst. The active material is promoted ruthenium metal, and the carrier is magnesium oxide.

Description

technical field [0001] The present invention relates to an improved catalyst active in the production of ammonia from ammonia synthesis gas. Furthermore, the present invention also relates to the recovery of useful catalytic components from spent catalysts. Background technique [0002] During the 20th century, the production of ammonia has increased significantly in terms of tonnage, so that ammonia ranks among the most important industrial chemical products. Today, more than 1% of global energy consumption is used for the production of ammonia by the traditional Haber-Borch process. Currently, multi-promoted iron catalysts are by far the most important catalysts used industrially. [0003] Recently, promoted ruthenium (Ru) catalysts supported on carbon have been introduced into commercial operations. A general disadvantage of ruthenium catalysts is the use of carbon supports under industrial conditions, since all forms of carbon are susceptible...

Claims

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Application Information

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IPC IPC(8): B01J20/34B01J23/00B01J23/46B01J23/58B01J23/63B01J23/96B01J35/10B01J38/00B01J38/48B01J38/60B01J38/66C01C1/04C01F1/00C01G55/00C22B7/00C22B11/00
CPCB01J23/96B01J23/63C01C1/0411B01J23/462C22B7/009Y10S502/514B01J23/58C22B11/048Y02P20/584Y02P20/52Y02P10/20
Inventor M·穆勒O·欣里希森H·比拉瓦C·J·H·雅格布森
Owner HALDOR TOPSOE AS
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