Method for preparing palladium nitrate

A technology of palladium nitrate and concentrated nitric acid, applied in chemical instruments and methods, ruthenium/rhodium/palladium/osmium/iridium/platinum compounds, inorganic chemistry, etc., can solve problems such as slow dissolution speed, consumption of concentrated nitric acid, etc., and achieve dissolution The effect of increased speed, low production cost and simple preparation steps

Inactive Publication Date: 2012-01-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Concentrated nitric acid dissolution method, the dissolution rate is slow, especially for metal palladium blocks, it takes a lot of concentrated nitric acid and takes a long time

Method used

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  • Method for preparing palladium nitrate

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Experimental program
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Effect test

Embodiment 1

[0018] Get 100 grams of sponge palladium powder with a purity > 99.95%, put it into a 2-liter beaker, add 300 grams of concentrated nitric acid with a weight concentration of 65% and 250 grams of hydrogen peroxide with a weight concentration of 30% slowly in two batches, each batch is Add concentrated nitric acid slowly first, and then add hydrogen peroxide immediately after the addition. The amount of the two added each time is 1 / 2 of the total amount. Heat the solution on an electric heater to 45°C. After dissolving, cool to room temperature and filter, then heat The solution was evaporated and concentrated to a slightly boiling state until a layer of crystal film appeared on the liquid surface, cooled and crystallized, and the obtained brown crystals were washed with deionized water at 6°C until there was no free nitric acid. Then put it into a vacuum oven with a vacuum degree of 0.05MPa, and dry it at 50°C for 8 hours, and the product [Pd(NO 3 ) 2 · 2H 2 O] After passin...

Embodiment 2

[0020] Get 150 grams of sponge palladium powder with a purity > 99.95%, put it into a 2-liter beaker, add 600 grams of concentrated nitric acid with a weight concentration of 65% and 300 grams of hydrogen peroxide with a weight concentration of 30% slowly in three batches, each batch is Add concentrated nitric acid slowly first, then add hydrogen peroxide immediately after the addition, the amount of the two added each time is one-third of the total, heat the solution on an electric heater to 50°C, after dissolving, cool to room temperature and filter, heat The solution was evaporated and concentrated to a slightly boiling state until a layer of crystal film appeared on the liquid surface, cooled and crystallized, and the obtained brown crystals were washed with 8°C deionized water until there was no free nitric acid. Then put it into a vacuum oven with a vacuum degree of 0.05MPa, and dry it at 50°C for 8 hours, and the product [Pd(NO 3 ) 2 · 2H 2 O] After passing the test,...

Embodiment 3

[0022] Get 100 grams of metal palladium blocks with a purity > 99.95%, put them into a 2-liter beaker, add 700 grams of concentrated nitric acid with a weight concentration of 68% and 600 grams of hydrogen peroxide with a weight concentration of 28% slowly in four batches, each batch is Add concentrated nitric acid slowly first, and then add hydrogen peroxide immediately after the addition. The amount of the two added each time is 1 / 4 of the total amount. Heat the solution on an electric heater to 55°C. After dissolving, cool to room temperature and filter, then heat The solution was evaporated to a slightly boiling state until a layer of crystal film appeared on the liquid surface, cooled and crystallized, and the obtained brown crystals were washed with deionized water at 5°C until no free nitric acid was present. Then put it into a vacuum oven with a vacuum degree of 0.06MPa, and dry it at 55°C for 7 hours, and the product [Pd(NO 3 ) 2 · 2H 2 O] After passing the test, t...

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Abstract

The invention discloses a method for preparing palladium nitrate, which comprises the following steps of: putting high-purity metal palladium or sponge palladium into a container, slowly adding concentrated nitric acid and hydrogen peroxide by batches, and heating for dissolution; cooling and filtering the solution, heating for evaporating and concentrating until solid-state crystal grains appear on liquid surface, and cooling for crystallization; and washing the obtained crystals with cold water, performing vacuum drying, and grinding into powder to obtain the palladium nitrate product. Compared with the prior art, the method has the advantages that: the concentrated nitric acid and the hydrogen peroxide are added slowly by batches in the dissolving process, the palladium dissolving capacity is improved, the reaction speed is improved, the using amount of the concentrated nitric acid is reduced, steps are simple, the efficiency is high, the production cost is low, and the palladium nitrate contains crystal water, has homogenous property and the purity close to 100 percent, and is a high-quality palladium nitrate product.

Description

technical field [0001] The invention relates to a preparation method of palladium nitrate. Background technique [0002] Palladium nitrate [Pd(NO 3 ) 2 · 2H 2 O] is used as a water-soluble palladium salt, mainly used in the preparation of other palladium-containing compounds, heterogeneous catalysts, etc. Traditional methods include aqua regia dissolution method and concentrated nitric acid dissolution method. The aqua regia dissolution method has a fast dissolution rate, but the chlorine needs to be driven out, and the process is complicated. Concentrated nitric acid dissolution method, the dissolution rate is slow, especially the metal palladium block, it needs to consume a large amount of concentrated nitric acid and takes a long time. Contents of the invention [0003] Aiming at the deficiencies in the prior art, the invention provides a method for preparing palladium nitrate which is short in time, easy to operate and low in production cost. [0004] The prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
Inventor 宋丽芝艾抚宾王海波勾连科薛冬
Owner CHINA PETROLEUM & CHEM CORP
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