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Method for preparing ruthenium nitrosyl nitrate solution

A technology of ruthenium nitrosyl nitrate and nitric acid aqueous solution, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve the problem of large reaction mass transfer resistance, nitrosylation Low degree, increased preparation complexity and other issues, to achieve a high degree of nitrosylation, improve the degree of nitrosylation of ruthenium, and low chlorine content

Active Publication Date: 2020-12-29
中国船舶集团有限公司第七一八研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

One is to directly feed NO into the reaction solution x (x=1,2) gas or pass into water to generate nitrous acid and then add to reaction liquid again, as CN106698529A, CN104556250A, this bubbling reaction, reaction mass transfer resistance is big, and the nitrosylation degree of ruthenium is low
In addition, this method requires an additional device on site to produce NO x gas, which increases the complexity of the preparation
The second way is to add nitrite to the reaction solution, and use it to react with acid to produce NO x Nitrosylation of gas, such as CN102616868A, CN102167405A, this method and the first method all belong to the external introduction of "NO x source", although the degree of nitrosylation has improved, it is still not ideal
In addition, the reaction solution will also introduce a large amount of alkali metal ions, which need to be processed by increasing the number of steps or washing times, which brings the complexity of preparation

Method used

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  • Method for preparing ruthenium nitrosyl nitrate solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) adopt chlorine oxidative distillation method to make ruthenium tetroxide gas, pass into nitric acid massfraction then and carry out absorption reaction in the nitric acid aqueous solution (containing nitric acid 5000g) of 65%, reaction temperature is 80 ℃, when ruthenium ion absorption reaches in solution At about 1000 g, stop feeding ruthenium tetroxide gas to prepare ruthenium absorbing liquid. Use the inductively coupled plasma spectrometer (ICP) to measure the mass of ruthenium ion in the ruthenium absorption solution, denoted as M 1 , measured M 1 = 1023 g.

[0043] (2) Lower the temperature of the ruthenium absorption solution prepared in step (1) to room temperature, then use a water bath to further lower the temperature to 10°C, add 300g (10mol) of formaldehyde at a speed of 20mL / min under stirring conditions, and react for 10h after the addition, and prepare Nitrosyl-containing ruthenium absorption solution.

[0044] (3) In the ruthenium absorption solut...

Embodiment 2

[0047] (1) adopt chlorine oxidative distillation method to make ruthenium tetroxide gas, pass into nitric acid massfraction then and carry out absorption reaction in the nitric acid aqueous solution (containing nitric acid 3000g) of 45%, reaction temperature is 95 ℃, when ruthenium ion absorption reaches in solution At about 1000 g, stop feeding ruthenium tetroxide gas to prepare ruthenium absorbing liquid. Use ICP to measure the mass of ruthenium ions in the ruthenium absorption solution, denoted as M 1 , measured M 1 = 1056 g.

[0048] (2) Lower the temperature of the ruthenium absorbing solution prepared in step (1) to room temperature, then use a water bath to further cool down to 15°C, add an aqueous solution containing 540g (6mol) oxalic acid at a speed of 5mL / min under stirring, and complete the reaction 4h, the ruthenium absorption solution containing nitrosyl was prepared.

[0049] (3) In the nitrosyl-containing ruthenium absorption solution prepared in step (2), s...

Embodiment 3

[0052] (1) adopt chlorine oxidative distillation method to make ruthenium tetroxide gas, pass into nitric acid massfraction then and carry out absorption reaction in the nitric acid aqueous solution (containing nitric acid 8000g) of 50%, reaction temperature is 60 ℃, when ruthenium ion absorption reaches in solution At about 1000 g, stop feeding ruthenium tetroxide gas to prepare ruthenium absorbing liquid. Use ICP to measure the mass of ruthenium ions in the ruthenium absorption solution, denoted as M 1 , measured M 1 =989g.

[0053] (2) Lower the temperature of the ruthenium absorption solution prepared in step (1) to room temperature, then use a water bath to further lower the temperature to 5°C, add 1380g (30mol) of ethanol at a speed of 50mL / min under stirring, and react for 6h after adding, A ruthenium absorption solution containing nitrosyl was prepared.

[0054] (3) In the nitrosyl-containing ruthenium absorption solution prepared in step (2), slowly add an aqueous ...

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Abstract

The invention relates to a method for preparing a ruthenium nitrosyl nitrate solution, and belongs to the technical field of precious metal compound preparation. The method comprises: introducing ruthenium tetroxide gas into a nitric acid aqueous solution, and carrying out an absorption reaction to prepare a ruthenium absorption liquid; adding a reducing agent into the ruthenium absorption liquid,and reacting at 5-15 DEG C to obtain a ruthenium absorption liquid containing nitrosyl; adding a pH regulator A, regulating the pH value to 5-7, adding a pH regulator B, regulating the pH value to 8-10 to obtain a ruthenium precipitate, and repeatedly filtering and washing to remove impurities; and adding a nitric acid aqueous solution, and carrying out a reflux reaction for more than 2 hours toobtain a ruthenium nitrosyl nitrate solution; According to the invention, the ruthenium nitrosyl nitrate solution prepared by the method has the characteristics of low chlorine content, low nitric acid content, low metal impurity content, low corrosion and high stability.

Description

technical field [0001] The invention relates to a method for preparing ruthenium nitrosyl nitrate solution, which belongs to the technical field of preparation of noble metal compounds. Background technique [0002] Ruthenium nitrosyl nitrate is mainly used to prepare electrodes and catalysts in the chemical industry, such as active cathodes in the chlor-alkali industry, ammonia synthesis catalysts, ammonia decomposition catalysts, and some industrial hydrogenation catalysts. Since the ruthenium nitrosyl nitrate product does not contain or only contains a small amount of chlorine, it has two obvious advantages in application compared with the basic compound of ruthenium, ruthenium trichloride: one is the counter electrode substrate, the catalyst carrier, and the carrier. The corrosivity of the device and equipment is significantly reduced; the second is that there will be no phenomenon that chlorine element inhibits the performance of electrodes and catalysts, and the activi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
CPCC01G55/00
Inventor 汤卫华张泰基郝刘仓赵丽娟刘妮张明
Owner 中国船舶集团有限公司第七一八研究所
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