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Ruthenium-based ammonia synthetic catalyst and preparation thereof

A catalyst, a technology for ammonia synthesis, which is used in the preparation/separation of ammonia, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve the problems of unfavorable catalyst use and promotion, expensive and other problems, and achieves low energy consumption and easy operation. , the effect of strong catalytic activity

Inactive Publication Date: 2008-12-17
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses Mg(OEt) 2 Prepare magnesium gel with ammonia water, and then use the impregnation method to load ruthenium carbonyl on the gel to prepare a catalyst with a high specific surface, with a specific surface as high as 290-359m 2 / g, which is 4 to 7 times that of commercial magnesium oxide, but due to Mg(OEt) 2 and Ru 3 (CO) 12 Precursors are relatively expensive precursors, which is not conducive to the use and promotion of catalysts
Directly prepare the method of ruthenium / magnesium oxide catalyst by co-precipitation of ruthenium chloride and magnesium nitrate has not been reported

Method used

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  • Ruthenium-based ammonia synthetic catalyst and preparation thereof
  • Ruthenium-based ammonia synthetic catalyst and preparation thereof
  • Ruthenium-based ammonia synthetic catalyst and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 25.6g magnesium nitrate and 0.43g ruthenium chloride (based on the mass of magnesium oxide carrier, containing 4% ruthenium, without special instructions, the percentages mentioned in the present invention are all percentages by weight) are mixed with 100ml mixed solution, after stirring for 10min , quickly add 100ml 2mol·L -1 In potassium hydroxide solution, stir for 5 minutes after adding, then wash with deionized water until there is no chloride ion, dry at 120°C for 24 hours, and then sinter at 450-550°C for 2 hours in a hydrogen-argon mixed gas atmosphere. The equal-volume impregnation method is used to impregnate the barium nitrate (M1) first, then the cesium nitrate (M2), and dry to prepare the Ru-M1-M2 / MgO catalyst.

[0026] Different series of ammonia synthesis catalysts Ru-M1 / MgO, Ru-M2 / MgO, Ru-M1-M2 / MgO can be prepared by changing the addition amount of ruthenium trichloride, additive amount and impregnation order, sintering reduction temperature Or impregna...

Embodiment 2

[0028] Catalyst activity evaluation was carried out in a high-pressure activity testing device. The reactor is a fixed bed with an inner diameter of 14mm. The catalyst particles are 12-16 meshes, the bulk volume is 2ml, and the catalyst is packed in the isothermal zone of the reactor. The reaction gas is a mixture of nitrogen and hydrogen, and the ratio of hydrogen to nitrogen is 3:1.

Embodiment 3

[0030] For Ru-Ba / MgO catalyst, the sintering temperature is 550°C, the sintering time is 2 hours, and the reaction gas space velocity is 10000h -1 , and the reaction pressure was 10MPa, the effect of reaction temperature on catalyst activity was investigated, and the results are shown in Table 1.

[0031] The influence (vol%) of table 1 reaction temperature on outlet ammonia concentration

[0032]

[0033] Note: The mark Ru4-Ba3 / MgO refers to the ruthenium catalyst containing 4% metal ruthenium and 3% metal barium on the ruthenium catalyst supported by magnesium oxide, and the following marks have the same meaning.

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Abstract

The invention provides a Ru-based ammonia synthesis catalyst and a preparation method thereof. The catalyst takes magnesium oxide as a carrier, metal ruthenium as an active constituent and at least one of alkali metal, alkaline earth metal or rare earth metal as an assistant; the composition is Ru-M1 / MgO, Ru-M2 / MgO, Ru-M1-M2 / MgO or Ru-(M1+M2) / MgO and the preparation method is as follows: the precursor, Ru-magnesium hydroxide catalyst, is prepared by a coprecipitation and dipping method: magnesium nitrate and ruthenium chloride are dissolved in water; the mixed solution is added into an alkaline solution to generate a precipitation; the precipitation is centrifugally washed, dried, sintered by reduction or soaked by equivoluminal soaking auxiliary after sintering, thus obtaining the catalyst that is required. The catalyst prepared by the synthesis method of the invention has good performance, relatively cheap raw material that is required, low energy consumption as well as simple devices and flow; besides, the catalyst is beneficial to reducing the cost and realizing mass production.

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 and a preparation method thereof. Background technique [0002] Ammonia synthesis catalyst is the most important catalyst in ammonia synthesis industry. In the 1980s and 1990s, people have studied the application of various oxides in ruthenium-based ammonia synthesis catalysts. Some early literatures introduced the research results of this part: that is, the ammonia synthesis activity of ruthenium catalysts is generally comparable to that of carrier oxides. The basicity (electronegativity) of the carrier is related, the higher the basicity of the carrier (the smaller the electronegativity), the better the activity of the catalyst, such as 673K, 80kPa, with Ru 3 (CO) 12 The ammonia synthesis activity order of the ruthenium catalyst prepared for the precursor is as follows: Ru / MgO>Ru / Ca...

Claims

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Application Information

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IPC IPC(8): B01J23/58C01C1/04
CPCY02P20/52
Inventor 魏可镁倪军王榕林建新俞秀金林炳裕
Owner FUZHOU UNIV
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