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Preparation method of hydrous ruthenium dioxide for resistance slurry

A resistance paste, ruthenium dioxide technology, applied in chemical instruments and methods, inorganic chemistry, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, etc. problems such as large expenses and equipment costs, to achieve the effect of uniform particle size, easy operation and low equipment requirements

Active Publication Date: 2016-01-27
中船黄冈贵金属有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, industrial production mainly uses alkali-dissolution-distillation, high temperature, chlorination-hydrolysis, etc. Among them, the alkali-dissolution-distillation method requires the use of highly corrosive molten salts (generally alkaline molten salts of alkali metal peroxides) Salt), not only requires special materials for electrodes and electrolytic cells, but also requires special technology for molten salt electrolysis, which requires a lot of money and equipment costs
[0008] At the same time, all current industrial production methods will produce toxic and explosive RuO 4 Vapor, causing potential hazards and process complexity in experiments or production processes

Method used

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  • Preparation method of hydrous ruthenium dioxide for resistance slurry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] First weigh 1.003g of ruthenium trichloride, dissolve it in 100mL of deionized water and mix evenly to make a solution, then add 0.3mL of hydrochloric acid with a mass fraction of 37% dropwise into the solution, and heat and stir with a constant temperature magnetic stirrer to make the trichloride The ruthenium chloride is hydrolyzed into a ruthenium chloride solution for use.

[0026] Weigh 0.8g of sodium hydroxide, dissolve it in 100mL of deionized water and mix well to make a sodium hydroxide solution.

[0027] Next, slowly pour the prepared ruthenium chloride solution into the sodium hydroxide solution until a large amount of black flocculent precipitates appear in the solution, then stop adding the ruthenium chloride solution, and then add hydrochloric acid solution dropwise to adjust the pH to neutral. There will be obvious solid-liquid delamination, pour off the supernatant, and filter the remaining solution through a sand core funnel. Repeatedly add hot water to...

Embodiment 2

[0031] First weigh 1.003g of ruthenium trichloride, dissolve it in 100mL of deionized water and mix evenly to make a solution, then add 0.3mL of hydrochloric acid with a mass fraction of 37% dropwise into the solution, and heat and stir with a constant temperature magnetic stirrer to make chlorine Ruthenium acid solution.

[0032] Weigh 0.73g sodium hydroxide, dissolve it in 100mL deionized water and mix well to make a solution

[0033] Next, slowly pour the chlororuthenic acid solution into the sodium hydroxide solution, stop adding the chlororuthenic acid solution until a large amount of black flocculent precipitates appear in the solution, then add the hydrochloric acid solution dropwise to adjust the pH to neutral, suction filter, and use hot water to Wash and dry in an oven at 90°C to obtain ultrafine hydrated ruthenium dioxide.

Embodiment 3

[0035] First weigh 100.0g of ruthenium trichloride, dissolve it in 1000mL of deionized water and mix evenly to make a solution, then add 30mL of hydrochloric acid with a mass fraction of 37% dropwise into the solution, and heat and stir with a constant temperature magnetic stirrer to make ruthenium chloride acid solution. At the same time, weigh 80g of sodium hydroxide, dissolve it into 1000mL of deionized water and mix it evenly to make a solution; then slowly pour the chlororuthenic acid solution into the sodium hydroxide solution until a large amount of black flocculent precipitates appear in the solution, then stop adding Chlororuthenic acid solution, then add hydrochloric acid solution dropwise to adjust the pH to 6-7, the reaction temperature is 60°C, use a sand core funnel to filter, wash with hot deionized water, place in a 90°C oven, and turn the sand core funnel upside down After drying, the superfine hydrated ruthenium dioxide can be obtained.

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Abstract

The invention discloses a preparation method of hydrous ruthenium dioxide for a resistance slurry. The method comprises the following steps: weighing a certain amount of a ruthenium source, adding a certain amount of hydrochloric acid to hydrolyze the ruthenium source into a ruthenium hydrochloride solution, adding the obtained ruthenium hydrochloride solution into a prepared sodium hydroxide solution in a dropwise manner until a black flocculent precipitate appears, adding hydrochloric acid to hydrolyze and neutralize, standing, carrying out pumping filtration, washing, and drying to prepare ultrafine hydrous ruthenium dioxide. The hydrous ruthenium dioxide prepared through the method has the advantages of high purity, uniform particle size, realization of the particle size control through adjusting technological conditions, and good dispersibility; and the method has the advantages of mild synthesis conditions, safety, reliability, simple process, simple operation, short cycle, high efficiency, low device requirements, and easy industrial large-scale production of ultrafine hydrous ruthenium dioxide powder.

Description

technical field [0001] The invention relates to a conductive phase material in a resistance slurry, in particular to a preparation method of a high-purity hydrated ruthenium dioxide material for a ruthenium-based resistance slurry. Background technique [0002] Due to its high resistance stability and wide resistance range, ruthenium dioxide has long been known as the conductive phase of thick film resistor paste. There are many ways to prepare ruthenium dioxide, such as electrodeposition method, sol-gel method, co-deposition method and so on. [0003] In 1995, Zheng et al. (ZhengJP, CyganPJ, JewTR. Hydrous ruthenium oxide as an electrode material for electrochemical capacitors [J]. J. Electrochem Soc., 1995, 142: 2699-2703) successfully prepared amorphous hydrated ruthenium dioxide in aqueous solution by sol-gel method. [0004] In 2000, TakasuY et al. (TakasuYandMurakamiY.Designofoxideelectrodeswithlargesurfacearea[J].Electrochim.Acta, 2000,45(25-26):4135-4141.) prepared ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
Inventor 刘显杰孙立志徐磊彭戴孙宝
Owner 中船黄冈贵金属有限公司
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