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Method for preparing ruthenium trichloride from coarse ruthenium powder

A technology of ruthenium trichloride and ruthenium powder, which is applied in the field of preparing ruthenium trichloride from coarse ruthenium powder, can solve the problems of many times of distillation and long time, difficult control of product quality, low product yield, etc. The effect of easy quality control and high product yield

Inactive Publication Date: 2010-11-24
CHENZHOU GAOXIN PLATINUM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, most of the preparation of ruthenium trichloride is obtained by oxidative distillation in alkaline medium or in sulfuric acid medium with pure ruthenium powder as the starting material, and the ruthenium absorption solution is obtained by concentration, crystallization and drying, while coarse ruthenium powder is used as the starting material The preparation of ruthenium trichloride has problems such as complex process, high energy consumption, heavy corrosion equipment, multiple distillation times and long time, difficult control of product quality, low product yield (up to 88%) and environmental pollution.

Method used

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  • Method for preparing ruthenium trichloride from coarse ruthenium powder
  • Method for preparing ruthenium trichloride from coarse ruthenium powder
  • Method for preparing ruthenium trichloride from coarse ruthenium powder

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Take 50g of coarse ruthenium powder (60.56% ruthenium content) in one or two mixtures of dilute sulfuric acid, ammonium chloride, hydrochloric acid or ammonia water medium with a mass fraction of 1-15%, and activate it to 200 After -800 mesh, filter and wash until neutral, put it into reactor a, add 0.5L NaOH solution with a mass fraction of 10–40%, add 2L of dilute sulfuric acid, dilute nitric acid or deionized water to the impurity removal bottles b and c One or several substances, the mass fraction of dilute sulfuric acid and dilute nitric acid solution is 0.1–5%, to Add 2.5L of 2–10mol / L hydrochloric acid and one or two mixtures of methanol, ethanol, n-propanol, and isopropanol to absorption bottles d, e, and f to keep the mass fraction at 0.01–6%. Add 3L of 5–10% NaOH solution to g. First turn on the vacuum pump h, close the purge valve i, check the airtightness of the entire preparation system, and adjust the negative pressure to 0.01–0.1MPa.

[0030] After fee...

Embodiment 2

[0032] Take 50g of coarse ruthenium powder (the ruthenium content is 76.50%) in one or two mixtures of dilute sulfuric acid, ammonium chloride, hydrochloric acid or ammonia water medium with a mass fraction of 1-15%, and activate it to 200 After -800 mesh, filter and wash until neutral, put it into reactor a, add 0.8L NaOH solution with a mass fraction of 10–40%, add 2L of dilute sulfuric acid, dilute nitric acid or deionized water to the impurity removal bottles b and c One or several substances, the mass fraction of dilute sulfuric acid and dilute nitric acid solution is 0.1–5%, to Add 2.5L of 2–10mol / L hydrochloric acid and one or two mixtures of methanol, ethanol, n-propanol, and isopropanol to absorption bottles d, e, and f to keep the mass fraction at 0.01–6%. Add 3L of 5–10% NaOH solution to g. First turn on the vacuum pump h, close the purge valve i, check the airtightness of the entire preparation system, and adjust the negative pressure to 0.01–0.1MPa.

[0033] Af...

Embodiment 3

[0035] Take 50g of coarse ruthenium powder (the ruthenium content is 90.16%) in one or two mixtures of dilute sulfuric acid, ammonium chloride, hydrochloric acid or ammonia water medium with a mass fraction of 1-15%, and activate it to 200 After -800 mesh, filter and wash until neutral, put it into reactor a, and add 1L of NaOH solution with a mass fraction of 10–40%, add 2L of dilute sulfuric acid, dilute nitric acid or deionized water to the impurity removal bottles b and c One or more substances, the mass fraction of dilute sulfuric acid and dilute nitric acid solution is 0.1–5%, to Add 2.5L of 2–10mol / L hydrochloric acid and one or two mixtures of methanol, ethanol, n-propanol, and isopropanol to absorption bottles d, e, and f to keep the mass fraction at 0.01–6%. Add 3L of 5–10% NaOH solution to g. First turn on the vacuum pump h, close the purge valve i, check the airtightness of the entire preparation system, and adjust the negative pressure to 0.01–0.1MPa.

[0036] A...

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Abstract

The invention discloses a method for preparing ruthenium trichloride from coarse ruthenium powder, which comprises the following steps: (1) grinding and activating the coarse ruthenium powder to 200-800 meshes by a high-frequency grinding machine in the presence of a dilute sulphuric acid, ammonium chloride, hydrochloric acid or ammonia water medium; filtering and washing the ground ruthenium powder to neutrality; adding deionized water to the neutral powder for slurrying; adding a proper amount of NaOH solution with a mass percent of 10-40% to the slurried powder under a negative pressure in a closed state; (2) heating to increase the temperature; introducing chlorine to the product obtained in step (1); controlling the reaction temperature between 80-105 DEG C to generate a yellow RnO4 gas; (3) introducing the RnO4 gas generated in step (2) to an impurity-removing absorbing liquid, and then introducing to a multi-level hydrochloric acid absorbing liquid; keeping the temperature of the absorbing liquid between 15-25 DEG C to generate a red brown H2RuCl5 solution by the reaction; and (4) performing heating, concentration, crystallization and infrared drying on the H2RuCl5 solution generated in step (3) to obtain a black brown RnCl3 crystal. The method has the advantages of simple process, low energy consumption, environment protection, little equipment corrosion, few distillation times, short reaction time, easy control of product quality and high product yield over 98%.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for preparing ruthenium trichloride from coarse ruthenium powder. Background technique [0002] The melting point of ruthenium is 2427 , insoluble in various acids, including aqua regia, but can be melted with caustic alkali and sodium peroxide; react with sulfuric acid solution of sodium hypochlorite (Chinese patent, publication number: CN101462778A), etc. [0003] Ruthenium trichloride is an important noble metal inorganic compound, which can form complexes with other reagents, and can also be used as a catalyst for isomerization, polymerization, hydrogenation and other reactions of organic matter, and can be used as an active catalyst for electrode coatings. It can also be used in the manufacture of chlororuthenate and the determination of sulfite, etc. [0004] At present, most of the preparation of ruthenium trichloride is obtained by oxidative...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
Inventor 雷婧冯志杰杨静杨拥军
Owner CHENZHOU GAOXIN PLATINUM
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