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Method of preparing ruthenium nitrosyl nitrate

A technology of ruthenium nitrosyl nitrate and sodium nitrite, which is applied in the field of directly preparing ruthenium nitrosyl nitrate with metal ruthenium powder, can solve the problems of high acidity, hindrance to application, high price, etc., and achieve simplified synthesis steps, shortened reaction time, The effect of improving reaction efficiency

Active Publication Date: 2017-07-07
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since this active precursor contains a large amount of chloride ions, the residual chloride ions on the catalyst cannot be completely removed during the catalyst preparation process, which has a certain inhibitory effect on the catalytic performance; at the same time, it was found that the halogen-free ruthenium precursor compound Such as Ru(NO)(NO 3 ) 3 and Ru 3 (CO) 12 It is an ideal precursor for the preparation of supported ruthenium catalysts, but the high price of this type of compound hinders its application in industry
[0003] However, the vast majority of ruthenium nitrosyl nitrate sold on the market is the nitric acid solution of ruthenium nitrosyl nitrate, and the introduction of nitrosyl group is not complete, which makes the prepared ruthenium nitrosyl nitrate unstable, and can only exist stably under acidic conditions. , part of the ruthenium nitrosyl nitrate will be decomposed into metal ruthenium after being concentrated into solid
And this solution acidity is higher, is unfavorable for the preparation of supported ruthenium catalyst, also can influence the catalytic activity of catalyst simultaneously

Method used

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  • Method of preparing ruthenium nitrosyl nitrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 5.0 g of ruthenium powder and 1.23 g of vanadium pentoxide and place them in a porcelain crucible, then put them in a microwave oven; feed air and keep the air velocity at 4000m 3 h -1 , calcined under 1000W microwave power for 15min, and then calcined under 1400W microwave power for 100min to oxidize metal ruthenium powder; the produced RuO 4 The gas is sequentially introduced into three absorption bottles containing 27.7g of nitric acid solution with a mass concentration of 45%, and the temperature of the nitric acid solution is controlled at 70°C to obtain Ru(NO 3 ) 3 acid solution.

[0018] The above obtained Ru(NO 3 ) 3 The acid solution was placed in a double-neck round bottom flask, and 5.12g of NaNO was slowly added 2 powder, stirred and heated at 80°C and condensed to reflux for 6 hours, the color of the solution gradually changed to deep red black, cooled the solution, and placed it in a separatory funnel, added 83mL of anhydrous ether for extractio...

Embodiment 2

[0020] Weigh 10.0 g of ruthenium powder and 2.4 g of vanadium pentoxide and place them in a porcelain crucible, then put them into a microwave oven, and feed air to keep the air velocity at 4500m 3 h -1 , calcined at 1000W microwave power for 17min, and then calcined at 1500W microwave power for 80min to oxidize metal ruthenium powder. will produce RuO 4 The gas is sequentially introduced into three absorption bottles containing 56.0 g of nitric acid solution with a mass concentration of 50%, and the temperature of the nitric acid solution is controlled at 70°C to obtain Ru(NO 3 ) 3 acid solution.

[0021] The above obtained Ru(NO 3 ) 3 The acid solution is all placed in a double-neck round bottom flask, slowly add 14.7g of KNO 2 powder, stirred and heated to reflux at 80°C for 7 hours, the color of the solution gradually turned dark red and black, cooled the solution, and placed it in a separatory funnel, added 168 mL of anhydrous ether for extraction 4 times, collected...

Embodiment 3

[0023] Weigh 15.0 g of ruthenium powder and 3.86 g of vanadium pentoxide and place them in a porcelain crucible, then put them in a microwave oven, and feed air to keep the air flow rate at 5000 m 3 h -1 , calcined under 1000W microwave power for 19min, and then calcined under 1600W microwave power for 60min to oxidize metal ruthenium powder. will produce RuO 4 The gas is sequentially introduced into three absorption bottles containing 85.1 g of nitric acid solution with a mass concentration of 55%, and the temperature of the nitric acid solution is controlled at 70°C to obtain Ru(NO 3 )3 acid solution.

[0024] The above obtained Ru(NO 3 ) 3 The acid solution was placed in a double-necked round bottom flask, and 20.5g of NaNO was slowly added 2 powder, stirred and heated to reflux at 80°C for 8 hours, the color of the solution gradually turned dark red and black, cooled the solution, and placed it in a separatory funnel, added 255 mL of anhydrous ether for extraction 3 t...

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Abstract

The invention discloses a method of preparing ruthenium nitrosyl nitrate. The method comprises the following steps: putting metal ruthenium powder and vanadium pentoxide (V2O5) in a ceramic crucible and then putting the crucible in a microwave oven; firstly, calcining the crucible for a while under 1000W power by microwaves, then calcining the crucible for a while under 1400-1600W power, introducing air to oxidize the metal ruthenium powder to generate ruthenium tetroxide gas, collecting gas and introducing the gas into a nitric acid solution, and then adding sodium nitrite to heat and performing reflux condensation; and adding a proper amount of anhydrous ether into a solution containing the ruthenium nitrosyl nitrate for extracting, and then evaporating ether to obtain a ruthenium nitrosyl nitrate solid. The method disclosed by the invention is easily available in raw material, high in product yield, simple to operate and convenient to treat. The obtained ruthenium nitrosyl nitrate does not contain halogens, and the product is high in purity and can be directly used for preparing a catalyst.

Description

technical field [0001] The invention relates to a synthesis method of a noble metal ruthenium catalyst, in particular to a method for directly preparing ruthenium nitrosyl nitrate with metal ruthenium powder. Background technique [0002] Supported ruthenium catalysts have good catalytic activity and are widely used in petrochemical, organic synthesis, environmental engineering, pharmaceutical engineering and other fields. Support, promoters and ruthenium active precursors are the main factors affecting the catalytic performance of supported ruthenium catalysts. The electronic structure of ruthenium is 4d 7 5s 1 , has the most oxidation states among all the elements in the periodic table, and each electronic structure has a variety of geometric structures, which provides a good basis for the synthesis of various ruthenium complexes. The active component ruthenium in the supported ruthenium catalyst is introduced through the ruthenium precursor compound. So far, the precu...

Claims

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Application Information

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IPC IPC(8): C01G55/00
CPCC01G55/00C01P2006/80
Inventor 高传柱白林奎刘清华杨波钱韵旭
Owner KUNMING UNIV OF SCI & TECH
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