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A new method for preparing ruthenium nitrosyl nitrate solution or pure crystal

A technology of ruthenium nitrosyl nitrate, nitric acid solution, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve the problems of volatile, human injury, cost rise and the like , to achieve the effect of simple equipment requirements, high product purity, and good promotion value

Active Publication Date: 2016-06-01
昆明铂生金属材料加工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method belongs to the category of pure synthetic chemical system, and has a wider scope of application than the first method, but it is the same as the problem faced by the patent CN102616868A, because a large amount of Na + , so it is essential to purify with ether (other organic solvents such as acetone can also be used), but ether is a highly volatile, flammable, and explosive chemical, and long-term or large-scale inhalation will cause considerable damage to the human body , will also cause adverse effects on the surrounding environment. Therefore, after the expansion of the scale, the issues of safety production and environmental protection are still the key issues to be considered. However, if a large amount of ether is used for extraction and distillation, corresponding equipment must be added, so the cost is also unreasonable. avoid rising

Method used

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  • A new method for preparing ruthenium nitrosyl nitrate solution or pure crystal
  • A new method for preparing ruthenium nitrosyl nitrate solution or pure crystal
  • A new method for preparing ruthenium nitrosyl nitrate solution or pure crystal

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Embodiment 1

[0042] 1) Prepare two 100ml flasks, each equipped with a double-hole rubber stopper and air guide tube, respectively put 10g of weighed copper flakes, 20g of lead nitrate powder, and the flask containing the copper flakes is equipped with a 100ml separating funnel .

[0043] 2) Slowly drop 5% HNO into the flask containing the copper piece through the separatory funnel 3 Solution, the flask containing lead nitrate powder is heated by an electric heater, and the gas generated after the reaction of the two flasks is introduced into 300ml of pure deionized water at 0-4°C prepared in advance through the catheter until there is no more gas in the two flasks Escaped, generated HNO 2 The solution was stored at low temperature until use.

[0044] 3) Weigh 2.66 g of RuCl 3 ·nH 2O solid, dissolved in 40ml of dilute nitric acid (5% concentration), poured into a 500ml three-neck round bottom flask, respectively equipped with reflux, heating, stirring devices and a separating funnel wit...

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Abstract

The invention discloses a new method for preparing a ruthenium nitrosyl nitrate solution or pure crystal, which comprises the following steps: 1. preparing a pure HNO2 solution; 2. dissolving commercially available RuCl3.nH2O in dilute nitric acid, gradually adding the HNO2 solution prepared in the step 1 under reflux conditions, and stirring until the solution completely becomes rose red, thereby obtaining an intermediate ruthenium nitrosyl chloride; 3. removing excess Cl<-> with an AgNO3 solution, and filtering to obtain a ruthenium nitrosyl nitrate nitric acid solution which conforms to the application requirements; and 4. drying the ruthenium nitrosyl nitrate nitric acid solution obtained in the step 3 by distillation to obtain the pure ruthenium nitrosyl nitrate solid. The method has the advantages of cheap and accessible raw materials, fewer steps and environment friendliness, does not need to design or use any special device, has wide application range (from laboratory small testing to industrial-scale generation), and has very high popularization value.

Description

technical field [0001] The invention relates to a ruthenium-based noble metal catalyst, in particular to a simple and efficient new method for preparing ruthenium nitrosyl nitrate (solution or pure crystal). Background technique [0002] As an important industrial catalyst, the ruthenium-based noble metal catalyst has gained more and more attention and application because of its lower price and better catalytic properties than other noble metal catalysts. Among them, ruthenium nitrosyl nitrate ( Structure Ru(NO)(NO 3 ) 3 ) as an important starting material for synthesis, and the commonly used RuCl 3 ·nH 2 O constitutes two major starting materials for the synthesis of ruthenium-based catalysts. [0003] Currently published ruthenium nitrosyl nitrate synthesis methods are divided into two categories: [0004] 1. Starting from industrial waste catalysts, RuO was prepared 4 or RuO 2 ·nH 2 O, absorb and reflux in nitric acid solution (CN101638727A, CN102616868A), if you ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G55/00
Inventor 王玉天孔令彦胡劲赵彦杰闭光育苏林赵娜王开军文劲松
Owner 昆明铂生金属材料加工有限公司
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